Synthesis and crystal structure of (3E,5S,10S,13S,14S,17Z)-17-ethylidene-10,13-dimethylhexadecahydro-3H-cyclopenta[α]phenanthren-3-one O-(methacryloyl) oxime, C50H74N2O4
Wei, Peng; Zhao, Jin-Feng; Zou, Juan; Ye, Jiang-Hai; He, Kang; Xu, Hong; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1219–1222; doi:10.1515/ncrs-2023-0413

data_8107707
_publ_section_title
;
 Synthesis and crystal structure of
 (3E,5S,10S,13S,14S,17Z)-17-ethylidene-10,13-dimethylhexadecahydro-3H-cyclopenta[\a]phenanthren-3-one
 O-(methacryloyl) oxime, C50H74N2O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1219
_journal_page_last               1222
_journal_paper_doi               10.1515/ncrs-2023-0413
_journal_volume                  238
_journal_year                    2023
_chemical_formula_sum            'C25 H37 N O2'
_chemical_formula_weight         383.55
_chemical_name_systematic
;
(3<i>E</i>,5<i>S</i>,10<i>S</i>,13<i>S</i>,14<i>S</i>,17<i>Z</i>)-17-ethylidene
-10,13-dimethylhexadecahydro-3<i>H</i>-cyclopenta[<i>\a</i>]phenanthren
-3-one <i>O</i>-(methacryloyl) oxime
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                99.1910(10)
_cell_angle_beta                 95.0390(10)
_cell_angle_gamma                95.8560(10)
_cell_formula_units_Z            2
_cell_length_a                   7.3320(3)
_cell_length_b                   11.8132(4)
_cell_length_c                   13.1604(5)
_cell_measurement_reflns_used    7491
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.6208
_cell_measurement_theta_min      3.0720
_cell_volume                     1113.06(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.10'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38222
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.590
_diffrn_reflns_theta_min         3.072
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       nubbly
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Flack x determined using 2663 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.8(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         18292
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                7800
_reflns_number_total             18292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0413_suppl_001.cif
_cod_data_source_block           A_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H74 N2 O4'
_cod_original_formula_weight         767.11
_cod_original_formula_units_Z            1
_cod_database_code               8107707
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              85728
_shelx_hkl_checksum              6322