The co-crystal structure of (17b)-estra-1,3,5(10)-triene-3,17diol – acetamide (1/1), a Z′ = 4 structure, C20H29NO3
Gong, Xiao F.; Song, Tao; Ning, Li F.; Chen, Xiao F.; Xu, Juan; Li, Peng; Gou, Ying Z.; Wang, Hui P.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 31–34; doi:10.1515/ncrs-2019-0451

data_8105006
_publ_section_title
;
 The co-crystal structure of (17b)-estra-1,3,5(10)-triene-3,17diol --
 acetamide (1/1), a Z&#x2032; = 4 structure, C20H29NO3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              31
_journal_page_last               34
_journal_paper_doi               10.1515/ncrs-2019-0451
_journal_volume                  235
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C18 H24 O2, C2 H5 N O'
_chemical_formula_sum            'C20 H29 N O3'
_chemical_formula_weight         331.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 108.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.167(3)
_cell_length_b                   9.3424(19)
_cell_length_c                   25.656(5)
_cell_measurement_reflns_used    11833
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      1.3264
_cell_volume                     3679.7(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25351
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         0.836
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 3845 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.4(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         15800
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.1030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+9.8105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2296
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.911
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                14183
_reflns_number_total             15800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0451_suppl.cif
_cod_data_source_block           bww19096
_cod_original_cell_volume        3679.8(14)
_cod_database_code               8105006
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O1(H1), O2(H2), O3(H3A), O4(H4), O5(H5), O6(H6A), O7(H7), O8(H8), N1(H1A,H1B),
  N4(H4A,H4B), N3(H3B,H3C), N2(H2B,H2C)
2.b Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C14(H14), C17(H17), C27(H27), C28(H28), C32(H32), C35(H35),
 C45(H45), C46(H46), C50(H50), C53(H53), C63(H63), C64(H64), C68(H68), C71(H71)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B),
 C16(H16A,H16B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B), C30(H30A,H30B),
  C33(H33A,H33B), C34(H34A,H34B), C43(H43A,H43B), C44(H44A,H44B), C47(H47A,
 H47B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,H52B), C61(H61A,H61B),
 C62(H62A,H62B), C65(H65A,H65B), C66(H66A,H66B), C69(H69A,H69B), C70(H70A,H70B)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C6(H6), C19(H19), C21(H21), C22(H22), C37(H37), C39(H39),
 C40(H40), C56(H56), C57(H57), C60(H60)
2.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C36(H36A,H36B,H36C), C54(H54A,H54B,H54C), C72(H72A,H72B,
 H72C), C74(H74A,H74B,H74C), C80(H80A,H80B,H80C), C78(H78A,H78B,H78C), C76(H76A,
 H76B,H76C)
;