 
data_MMW221_A_0ma
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C41 H47 N5 O4'
_chemical_formula_sum
 'C41 H47 N5 O4' 
_chemical_formula_weight          673.83

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            4
_space_group_name_H-M_alt         'P 21'
_space_group_name_Hall            'P 2yb'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    11.7353(5)
_cell_length_b                    10.8296(4)
_cell_length_c                    15.1159(6)
_cell_angle_alpha                 90
_cell_angle_beta                  93.981(3)
_cell_angle_gamma                 90
_cell_volume                      1916.42(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     4104 
_cell_measurement_theta_min       3.78 
_cell_measurement_theta_max       68.43 
 
_exptl_crystal_description        cubic 
_exptl_crystal_colour             colourless 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured'              
_exptl_crystal_density_diffrn     1.168          
_exptl_crystal_F_000              720
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.426
_exptl_crystal_size_mid           0.391
_exptl_crystal_size_min           0.228
_exptl_absorpt_coefficient_mu     0.605
_shelx_estimated_absorpt_T_min    0.783
_shelx_estimated_absorpt_T_max    0.874
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.7830 
_exptl_absorpt_correction_T_max   0.8740 
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             53770
_diffrn_reflns_av_unetI/netI      0.0487
_diffrn_reflns_av_R_equivalents   0.0840
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.776
_diffrn_reflns_theta_max          68.433
_diffrn_reflns_theta_full         67.679
_diffrn_measured_fraction_theta_max   0.981
_diffrn_measured_fraction_theta_full  0.988
_diffrn_reflns_Laue_measured_fraction_max    0.981
_diffrn_reflns_Laue_measured_fraction_full   0.988
_diffrn_reflns_point_group_measured_fraction_max   0.982
_diffrn_reflns_point_group_measured_fraction_full  0.989
_reflns_number_total              6754
_reflns_number_gt                 4104
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.893
_reflns_Friedel_fraction_max      0.983
_reflns_Friedel_fraction_full     0.990
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'
 
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1097P)²+0.2011P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    -0.1(5)
_chemical_absolute_configuration  'rm'
_refine_ls_number_reflns          6754
_refine_ls_number_parameters      472
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.1053
_refine_ls_R_factor_gt            0.0577
_refine_ls_wR_factor_ref          0.1927
_refine_ls_wR_factor_gt           0.1575
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.020
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
O1 O 0.2709(3) 0.5897(3) 0.9350(2) 0.0809(10) Uani 1 1 d . . . . .
O2 O 0.1499(2) 0.6278(3) 0.7684(2) 0.0770(9) Uani 1 1 d . . . . .
O3 O 0.2852(3) 0.6489(3) 0.6237(2) 0.0820(10) Uani 1 1 d . . . . .
O4 O 0.4685(3) 0.8983(3) 0.6560(2) 0.0835(10) Uani 1 1 d . . . . .
N1 N 0.4888(3) 0.7483(4) 0.8086(3) 0.0733(11) Uani 1 1 d . . . . .
H1A H 0.5360 0.8088 0.8161 0.088 Uiso 1 1 calc R U . . .
N2 N 0.5741(3) 0.5394(4) 0.9680(3) 0.0735(11) Uani 1 1 d . . . . .
N3 N 0.6047(4) 0.4187(4) 0.9620(3) 0.0842(12) Uani 1 1 d . . . . .
N4 N 0.5472(4) 0.3722(4) 0.8949(3) 0.0851(12) Uani 1 1 d . . . . .
N5 N 0.4794(4) 0.4602(4) 0.8551(3) 0.0836(12) Uani 1 1 d . . . . .
C1 C 0.4405(4) 0.6847(4) 0.8826(4) 0.0677(13) Uani 1 1 d . . . . .
C2 C 0.3100(4) 0.6719(4) 0.8701(3) 0.0658(12) Uani 1 1 d . . . . .
C3 C 0.2710(4) 0.6239(5) 0.7801(3) 0.0659(11) Uani 1 1 d . . . . .
C4 C 0.3216(4) 0.7003(5) 0.7082(3) 0.0667(12) Uani 1 1 d . . . . .
C5 C 0.4510(4) 0.7013(5) 0.7213(3) 0.0694(12) Uani 1 1 d . . . . .
C6 C 0.4973(4) 0.5629(4) 0.9009(3) 0.0664(12) Uani 1 1 d . . . . .
C7 C 0.6305(5) 0.6202(5) 1.0346(3) 0.0819(15) Uani 1 1 d . . . . .
H7 H 0.5863 0.6969 1.0358 0.098 Uiso 1 1 calc R U . . .
C8 C 0.7475(7) 0.6521(9) 1.0100(4) 0.130(3) Uani 1 1 d . . . . .
H8A H 0.7910 0.5770 1.0032 0.155 Uiso 1 1 calc R U . . .
H8B H 0.7426 0.6952 0.9536 0.155 Uiso 1 1 calc R U . . .
C9 C 0.8068(9) 0.7309(10) 1.0784(5) 0.154(4) Uani 1 1 d . . . . .
H9A H 0.7673 0.8095 1.0803 0.184 Uiso 1 1 calc R U . . .
H9B H 0.8837 0.7471 1.0617 0.184 Uiso 1 1 calc R U . . .
C10 C 0.8128(7) 0.6748(7) 1.1678(5) 0.118(2) Uani 1 1 d . . . . .
H10A H 0.8485 0.7320 1.2107 0.142 Uiso 1 1 calc R U . . .
H10B H 0.8587 0.6003 1.1682 0.142 Uiso 1 1 calc R U . . .
C11 C 0.6947(9) 0.6444(9) 1.1925(4) 0.133(3) Uani 1 1 d . . . . .
H11A H 0.6521 0.7204 1.1985 0.160 Uiso 1 1 calc R U . . .
H11B H 0.6993 0.6029 1.2495 0.160 Uiso 1 1 calc R U . . .
C12 C 0.6320(7) 0.5630(8) 1.1246(4) 0.113(2) Uani 1 1 d . . . . .
H12A H 0.6690 0.4830 1.1236 0.136 Uiso 1 1 calc R U . . .
H12B H 0.5542 0.5506 1.1406 0.136 Uiso 1 1 calc R U . . .
C13 C 0.2257(9) 0.6431(8) 1.0091(5) 0.146(3) Uani 1 1 d . . . . .
H13A H 0.1657 0.7009 0.9902 0.175 Uiso 1 1 calc R U . . .
H13B H 0.2850 0.6881 1.0435 0.175 Uiso 1 1 calc R U . . .
C14 C 0.1793(6) 0.5455(7) 1.0639(4) 0.0969(18) Uani 1 1 d . . . . .
C15 C 0.2388(9) 0.4776(15) 1.1278(7) 0.178(5) Uani 1 1 d . . . . .
H15 H 0.3160 0.4954 1.1392 0.214 Uiso 1 1 calc R U . . .
C16 C 0.191(2) 0.3813(19) 1.1783(11) 0.235(10) Uani 1 1 d . . . . .
H16 H 0.2299 0.3401 1.2253 0.282 Uiso 1 1 calc R U . . .
C17 C 0.086(2) 0.3593(14) 1.1489(10) 0.205(8) Uani 1 1 d . . . . .
H17 H 0.0534 0.2904 1.1741 0.246 Uiso 1 1 calc R U . . .
C18 C 0.0185(11) 0.4163(13) 1.0911(10) 0.173(4) Uani 1 1 d . . . . .
H18 H -0.0583 0.3963 1.0802 0.208 Uiso 1 1 calc R U . . .
C19 C 0.0703(7) 0.5081(9) 1.0478(6) 0.133(3) Uani 1 1 d . . . . .
H19 H 0.0268 0.5487 1.0030 0.159 Uiso 1 1 calc R U . . .
C20 C 0.1005(5) 0.5095(6) 0.7720(5) 0.1037(19) Uani 1 1 d . . . . .
H20A H 0.1144 0.4753 0.8311 0.124 Uiso 1 1 calc R U . . .
H20B H 0.1346 0.4549 0.7304 0.124 Uiso 1 1 calc R U . . .
C21 C -0.0272(4) 0.5200(6) 0.7488(4) 0.0870(16) Uani 1 1 d . . . . .
C22 C -0.0968(8) 0.4452(10) 0.7937(6) 0.136(3) Uani 1 1 d . . . . .
H22 H -0.0658 0.3928 0.8379 0.164 Uiso 1 1 calc R U . . .
C23 C -0.2147(11) 0.4475(16) 0.7733(11) 0.191(5) Uani 1 1 d . . . . .
H23 H -0.2631 0.3957 0.8023 0.229 Uiso 1 1 calc R U . . .
C24 C -0.2552(9) 0.5243(15) 0.7123(16) 0.213(8) Uani 1 1 d . . . . .
H24 H -0.3339 0.5285 0.7002 0.255 Uiso 1 1 calc R U . . .
C25 C -0.1874(10) 0.5983(11) 0.6657(9) 0.181(5) Uani 1 1 d . . . . .
H25 H -0.2188 0.6501 0.6214 0.217 Uiso 1 1 calc R U . . .
C26 C -0.0723(6) 0.5949(8) 0.6854(5) 0.121(2) Uani 1 1 d . . . . .
H26 H -0.0247 0.6452 0.6544 0.145 Uiso 1 1 calc R U . . .
C27 C 0.2238(7) 0.7287(7) 0.5650(4) 0.121(3) Uani 1 1 d . . . . .
H27A H 0.2764 0.7854 0.5394 0.145 Uiso 1 1 calc R U . . .
H27B H 0.1709 0.7768 0.5975 0.145 Uiso 1 1 calc R U . . .
C28 C 0.1602(5) 0.6615(7) 0.4938(4) 0.0963(18) Uani 1 1 d . . . . .
C29 C 0.1280(11) 0.5418(11) 0.5021(7) 0.179(5) Uani 1 1 d . . . . .
H29 H 0.1514 0.4986 0.5533 0.215 Uiso 1 1 calc R U . . .
C30 C 0.0610(14) 0.4826(15) 0.4360(10) 0.235(7) Uani 1 1 d . . . . .
H30 H 0.0392 0.4012 0.4447 0.282 Uiso 1 1 calc R U . . .
C31 C 0.0285(14) 0.536(2) 0.3636(10) 0.221(7) Uani 1 1 d . . . . .
H31 H -0.0248 0.4999 0.3234 0.266 Uiso 1 1 calc R U . . .
C32 C 0.0739(15) 0.648(3) 0.3470(8) 0.252(9) Uani 1 1 d . . . . .
H32 H 0.0658 0.6814 0.2902 0.302 Uiso 1 1 calc R U . . .
C33 C 0.1334(9) 0.7138(13) 0.4158(7) 0.186(5) Uani 1 1 d . . . . .
H33 H 0.1544 0.7954 0.4065 0.223 Uiso 1 1 calc R U . . .
C34 C 0.5072(5) 0.7756(5) 0.6515(4) 0.0841(15) Uani 1 1 d . . . . .
H34A H 0.5896 0.7726 0.6622 0.101 Uiso 1 1 calc R U . . .
H34B H 0.4871 0.7416 0.5931 0.101 Uiso 1 1 calc R U . . .
C35 C 0.5177(7) 0.9748(6) 0.5917(5) 0.122(2) Uani 1 1 d . . . . .
H35A H 0.5018 0.9409 0.5328 0.146 Uiso 1 1 calc R U . . .
H35B H 0.5998 0.9793 0.6038 0.146 Uiso 1 1 calc R U . . .
C36 C 0.4667(7) 1.0996(5) 0.5971(4) 0.0945(18) Uani 1 1 d . . . . .
C37 C 0.3576(8) 1.1229(7) 0.5628(4) 0.110(2) Uani 1 1 d . . . . .
H37 H 0.3142 1.0605 0.5349 0.132 Uiso 1 1 calc R U . . .
C38 C 0.3131(9) 1.2402(8) 0.5700(5) 0.132(3) Uani 1 1 d . . . . .
H38 H 0.2396 1.2563 0.5457 0.159 Uiso 1 1 calc R U . . .
C39 C 0.3730(12) 1.3314(8) 0.6110(6) 0.131(3) Uani 1 1 d . . . . .
H39 H 0.3401 1.4090 0.6154 0.157 Uiso 1 1 calc R U . . .
C40 C 0.4781(11) 1.3126(8) 0.6452(7) 0.142(3) Uani 1 1 d . . . . .
H40 H 0.5194 1.3765 0.6732 0.170 Uiso 1 1 calc R U . . .
C41 C 0.5260(7) 1.1959(9) 0.6388(6) 0.131(3) Uani 1 1 d . . . . .
H41 H 0.5999 1.1823 0.6632 0.158 Uiso 1 1 calc R U . . .
H2 H 0.273(4) 0.749(5) 0.878(3) 0.063(12) Uiso 1 1 d . . . . .
H3 H 0.296(3) 0.537(4) 0.771(2) 0.052(10) Uiso 1 1 d . . . . .
H5 H 0.475(3) 0.612(5) 0.716(3) 0.058(11) Uiso 1 1 d . . . . .
H4 H 0.290(3) 0.781(4) 0.713(2) 0.050(10) Uiso 1 1 d . . . . .
H1 H 0.456(4) 0.728(5) 0.923(3) 0.062(14) Uiso 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
O1 C13 1.397(7) . ?
O1 C2 1.424(6) . ?
O2 C20 1.408(7) . ?
O2 C3 1.421(5) . ?
O3 C27 1.402(6) . ?
O3 C4 1.430(6) . ?
O4 C34 1.407(6) . ?
O4 C35 1.429(7) . ?
N1 C5 1.454(6) . ?
N1 C1 1.462(7) . ?
N1 H1A 0.8600 . ?
N2 C6 1.334(6) . ?
N2 N3 1.360(6) . ?
N2 C7 1.457(6) . ?
N3 N4 1.282(6) . ?
N4 N5 1.355(6) . ?
N5 C6 1.320(6) . ?
C1 C6 1.495(7) . ?
C1 C2 1.535(7) . ?
C1 H1 0.79(5) . ?
C2 C3 1.499(7) . ?
C2 H2 0.95(5) . ?
C3 C4 1.519(7) . ?
C3 H3 1.00(4) . ?
C4 C5 1.518(7) . ?
C4 H4 0.95(5) . ?
C5 C34 1.514(8) . ?
C5 H5 1.01(5) . ?
C7 C8 1.488(9) . ?
C7 C12 1.493(8) . ?
C7 H7 0.9800 . ?
C8 C9 1.477(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.480(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.497(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.507(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.471(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C19 1.347(10) . ?
C14 C15 1.367(13) . ?
C15 C16 1.43(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.31(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.294(19) . ?
C17 H17 0.9300 . ?
C18 C19 1.357(14) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.520(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C26 1.335(9) . ?
C21 C22 1.365(10) . ?
C22 C23 1.397(15) . ?
C22 H22 0.9300 . ?
C23 C24 1.31(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.36(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.363(12) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.460(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C33 1.326(11) . ?
C28 C29 1.359(13) . ?
C29 C30 1.384(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.27(2) . ?
C30 H30 0.9300 . ?
C31 C32 1.35(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.41(2) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.482(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.371(9) . ?
C36 C41 1.382(11) . ?
C37 C38 1.380(11) . ?
C37 H37 0.9300 . ?
C38 C39 1.339(12) . ?
C38 H38 0.9300 . ?
C39 C40 1.319(13) . ?
C39 H39 0.9300 . ?
C40 C41 1.389(13) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C13 O1 C2 116.8(5) . . ?
C20 O2 C3 112.3(4) . . ?
C27 O3 C4 115.7(4) . . ?
C34 O4 C35 111.6(4) . . ?
C5 N1 C1 114.7(4) . . ?
C5 N1 H1A 122.6 . . ?
C1 N1 H1A 122.6 . . ?
C6 N2 N3 107.4(4) . . ?
C6 N2 C7 131.4(4) . . ?
N3 N2 C7 120.9(4) . . ?
N4 N3 N2 107.7(4) . . ?
N3 N4 N5 109.6(4) . . ?
C6 N5 N4 107.0(4) . . ?
N1 C1 C6 111.4(4) . . ?
N1 C1 C2 112.7(4) . . ?
C6 C1 C2 111.8(4) . . ?
N1 C1 H1 104(4) . . ?
C6 C1 H1 107(4) . . ?
C2 C1 H1 109(4) . . ?
O1 C2 C3 108.5(4) . . ?
O1 C2 C1 109.8(4) . . ?
C3 C2 C1 112.4(4) . . ?
O1 C2 H2 107(3) . . ?
C3 C2 H2 107(3) . . ?
C1 C2 H2 111(3) . . ?
O2 C3 C2 110.0(4) . . ?
O2 C3 C4 109.4(4) . . ?
C2 C3 C4 110.6(4) . . ?
O2 C3 H3 108(2) . . ?
C2 C3 H3 112(2) . . ?
C4 C3 H3 106(2) . . ?
O3 C4 C5 110.7(4) . . ?
O3 C4 C3 108.7(4) . . ?
C5 C4 C3 110.3(4) . . ?
O3 C4 H4 109(2) . . ?
C5 C4 H4 112(2) . . ?
C3 C4 H4 106(2) . . ?
N1 C5 C34 109.0(4) . . ?
N1 C5 C4 111.2(4) . . ?
C34 C5 C4 113.1(4) . . ?
N1 C5 H5 109(2) . . ?
C34 C5 H5 109(2) . . ?
C4 C5 H5 105(2) . . ?
N5 C6 N2 108.2(4) . . ?
N5 C6 C1 126.4(4) . . ?
N2 C6 C1 125.3(4) . . ?
N2 C7 C8 110.5(5) . . ?
N2 C7 C12 110.9(5) . . ?
C8 C7 C12 111.8(5) . . ?
N2 C7 H7 107.8 . . ?
C8 C7 H7 107.8 . . ?
C12 C7 H7 107.8 . . ?
C9 C8 C7 111.0(7) . . ?
C9 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 C10 113.1(7) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C11 109.4(6) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 112.1(6) . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C7 C12 C11 110.7(6) . . ?
C7 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
O1 C13 C14 109.2(6) . . ?
O1 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
O1 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
C19 C14 C15 113.4(9) . . ?
C19 C14 C13 119.9(8) . . ?
C15 C14 C13 126.4(9) . . ?
C14 C15 C16 124.8(13) . . ?
C14 C15 H15 117.6 . . ?
C16 C15 H15 117.6 . . ?
C17 C16 C15 110.3(14) . . ?
C17 C16 H16 124.8 . . ?
C15 C16 H16 124.8 . . ?
C18 C17 C16 131.4(19) . . ?
C18 C17 H17 114.3 . . ?
C16 C17 H17 114.3 . . ?
C17 C18 C19 113.7(13) . . ?
C17 C18 H18 123.1 . . ?
C19 C18 H18 123.1 . . ?
C14 C19 C18 125.8(11) . . ?
C14 C19 H19 117.1 . . ?
C18 C19 H19 117.1 . . ?
O2 C20 C21 109.0(5) . . ?
O2 C20 H20A 109.9 . . ?
C21 C20 H20A 109.9 . . ?
O2 C20 H20B 109.9 . . ?
C21 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
C26 C21 C22 119.8(7) . . ?
C26 C21 C20 123.1(6) . . ?
C22 C21 C20 117.0(7) . . ?
C21 C22 C23 119.8(10) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 118.3(12) . . ?
C24 C23 H23 120.8 . . ?
C22 C23 H23 120.8 . . ?
C23 C24 C25 122.9(11) . . ?
C23 C24 H24 118.5 . . ?
C25 C24 H24 118.5 . . ?
C24 C25 C26 118.5(12) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
C21 C26 C25 120.7(10) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
O3 C27 C28 112.0(6) . . ?
O3 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
O3 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C33 C28 C29 116.1(8) . . ?
C33 C28 C27 121.3(8) . . ?
C29 C28 C27 122.6(6) . . ?
C28 C29 C30 121.5(10) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C31 C30 C29 121.9(16) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 118.0(13) . . ?
C30 C31 H31 121.0 . . ?
C32 C31 H31 121.0 . . ?
C31 C32 C33 119.9(13) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C28 C33 C32 121.1(14) . . ?
C28 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
O4 C34 C5 108.1(4) . . ?
O4 C34 H34A 110.1 . . ?
C5 C34 H34A 110.1 . . ?
O4 C34 H34B 110.1 . . ?
C5 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
O4 C35 C36 108.0(5) . . ?
O4 C35 H35A 110.1 . . ?
C36 C35 H35A 110.1 . . ?
O4 C35 H35B 110.1 . . ?
C36 C35 H35B 110.1 . . ?
H35A C35 H35B 108.4 . . ?
C37 C36 C41 117.5(6) . . ?
C37 C36 C35 121.1(7) . . ?
C41 C36 C35 121.4(8) . . ?
C36 C37 C38 119.2(8) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C39 C38 C37 121.7(9) . . ?
C39 C38 H38 119.1 . . ?
C37 C38 H38 119.1 . . ?
C40 C39 C38 120.9(9) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 119.0(9) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
C36 C41 C40 121.6(9) . . ?
C36 C41 H41 119.2 . . ?
C40 C41 H41 119.2 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C6 N2 N3 N4 -0.9(6) . . . . ?
C7 N2 N3 N4 -175.9(4) . . . . ?
N2 N3 N4 N5 0.8(6) . . . . ?
N3 N4 N5 C6 -0.4(6) . . . . ?
C5 N1 C1 C6 77.1(5) . . . . ?
C5 N1 C1 C2 -49.5(5) . . . . ?
C13 O1 C2 C3 -137.1(6) . . . . ?
C13 O1 C2 C1 99.7(7) . . . . ?
N1 C1 C2 O1 169.0(4) . . . . ?
C6 C1 C2 O1 42.6(6) . . . . ?
N1 C1 C2 C3 48.2(6) . . . . ?
C6 C1 C2 C3 -78.3(5) . . . . ?
C20 O2 C3 C2 -106.7(5) . . . . ?
C20 O2 C3 C4 131.6(5) . . . . ?
O1 C2 C3 O2 65.3(5) . . . . ?
C1 C2 C3 O2 -173.1(4) . . . . ?
O1 C2 C3 C4 -173.7(4) . . . . ?
C1 C2 C3 C4 -52.1(5) . . . . ?
C27 O3 C4 C5 -117.6(6) . . . . ?
C27 O3 C4 C3 121.1(6) . . . . ?
O2 C3 C4 O3 -60.5(5) . . . . ?
C2 C3 C4 O3 178.1(4) . . . . ?
O2 C3 C4 C5 178.0(4) . . . . ?
C2 C3 C4 C5 56.6(5) . . . . ?
C1 N1 C5 C34 179.8(4) . . . . ?
C1 N1 C5 C4 54.4(5) . . . . ?
O3 C4 C5 N1 -177.5(4) . . . . ?
C3 C4 C5 N1 -57.2(5) . . . . ?
O3 C4 C5 C34 59.4(5) . . . . ?
C3 C4 C5 C34 179.7(4) . . . . ?
N4 N5 C6 N2 -0.2(6) . . . . ?
N4 N5 C6 C1 -179.3(5) . . . . ?
N3 N2 C6 N5 0.7(6) . . . . ?
C7 N2 C6 N5 175.0(5) . . . . ?
N3 N2 C6 C1 179.7(5) . . . . ?
C7 N2 C6 C1 -6.0(8) . . . . ?
N1 C1 C6 N5 -77.2(6) . . . . ?
C2 C1 C6 N5 49.9(7) . . . . ?
N1 C1 C6 N2 103.9(6) . . . . ?
C2 C1 C6 N2 -129.0(5) . . . . ?
C6 N2 C7 C8 -99.9(7) . . . . ?
N3 N2 C7 C8 73.7(6) . . . . ?
C6 N2 C7 C12 135.6(6) . . . . ?
N3 N2 C7 C12 -50.8(7) . . . . ?
N2 C7 C8 C9 -178.3(6) . . . . ?
C12 C7 C8 C9 -54.3(9) . . . . ?
C7 C8 C9 C10 56.2(12) . . . . ?
C8 C9 C10 C11 -56.2(11) . . . . ?
C9 C10 C11 C12 55.3(9) . . . . ?
N2 C7 C12 C11 177.6(6) . . . . ?
C8 C7 C12 C11 53.8(8) . . . . ?
C10 C11 C12 C7 -54.9(9) . . . . ?
C2 O1 C13 C14 174.3(6) . . . . ?
O1 C13 C14 C19 -88.2(10) . . . . ?
O1 C13 C14 C15 85.8(10) . . . . ?
C19 C14 C15 C16 -4.1(16) . . . . ?
C13 C14 C15 C16 -178.4(12) . . . . ?
C14 C15 C16 C17 6(2) . . . . ?
C15 C16 C17 C18 -8(3) . . . . ?
C16 C17 C18 C19 7(2) . . . . ?
C15 C14 C19 C18 2.8(12) . . . . ?
C13 C14 C19 C18 177.5(8) . . . . ?
C17 C18 C19 C14 -3.7(14) . . . . ?
C3 O2 C20 C21 -173.7(5) . . . . ?
O2 C20 C21 C26 39.3(9) . . . . ?
O2 C20 C21 C22 -143.1(7) . . . . ?
C26 C21 C22 C23 -0.1(13) . . . . ?
C20 C21 C22 C23 -177.8(9) . . . . ?
C21 C22 C23 C24 -1.5(19) . . . . ?
C22 C23 C24 C25 3(2) . . . . ?
C23 C24 C25 C26 -2(2) . . . . ?
C22 C21 C26 C25 0.7(12) . . . . ?
C20 C21 C26 C25 178.3(8) . . . . ?
C24 C25 C26 C21 0.3(15) . . . . ?
C4 O3 C27 C28 -162.0(5) . . . . ?
O3 C27 C28 C33 -153.9(9) . . . . ?
O3 C27 C28 C29 24.1(12) . . . . ?
C33 C28 C29 C30 -6.4(19) . . . . ?
C27 C28 C29 C30 175.5(12) . . . . ?
C28 C29 C30 C31 2(3) . . . . ?
C29 C30 C31 C32 9(3) . . . . ?
C30 C31 C32 C33 -14(3) . . . . ?
C29 C28 C33 C32 0.8(19) . . . . ?
C27 C28 C33 C32 178.9(13) . . . . ?
C31 C32 C33 C28 10(3) . . . . ?
C35 O4 C34 C5 -179.9(6) . . . . ?
N1 C5 C34 O4 -63.8(5) . . . . ?
C4 C5 C34 O4 60.4(6) . . . . ?
C34 O4 C35 C36 176.3(6) . . . . ?
O4 C35 C36 C37 -75.4(9) . . . . ?
O4 C35 C36 C41 103.0(7) . . . . ?
C41 C36 C37 C38 0.9(10) . . . . ?
C35 C36 C37 C38 179.4(6) . . . . ?
C36 C37 C38 C39 -1.1(12) . . . . ?
C37 C38 C39 C40 0.9(13) . . . . ?
C38 C39 C40 C41 -0.5(14) . . . . ?
C37 C36 C41 C40 -0.6(11) . . . . ?
C35 C36 C41 C40 -179.1(8) . . . . ?
C39 C40 C41 C36 0.4(14) . . . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C1 H1 N3  0.79(5) 2.82(5) 3.521(7) 150(4) 2_657
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C1 H1 N3  0.79(5) 2.82(5) 3.521(7) 150(4) 2_657
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C20 H20A O1  0.97 2.64 3.184(7) 115.7 .
C3 H3 N5  1.00(4) 2.56(4) 3.166(6) 119(3) .
C5 H5 N5  1.01(5) 2.66(4) 3.305(7) 121(3) .
 
_refine_diff_density_max    0.235
_refine_diff_density_min   -0.230
_refine_diff_density_rms    0.038

_shelxl_version_number 2014-3



