Synthesis and crystal structure of 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO
Zhao, Jin-Feng; Zhang, Wen-Wen; Ye, Jiang-Hai; He, Kang; Zou, Juan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 579–581; doi:10.1515/ncrs-2023-0105

data_8107500
_publ_section_title
;
 Synthesis and crystal structure of
 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[\a]phenanthren-17-yl)ethan-1-one,
 C28H41NO
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              579
_journal_page_last               581
_journal_paper_doi               10.1515/ncrs-2023-0105
_journal_volume                  238
_journal_year                    2023
_chemical_formula_sum            'C28 H41 N O'
_chemical_formula_weight         407.62
_chemical_name_systematic
;
1-((3<i>R</i>,10<i>S</i>,13<i>S</i>,17<i>S</i>)-10,13-
dimethyl-3-(m-tolylamino)hexadecahydro-1<i>H</i>-
cyclopenta[<i>\a</i>]phenanthren-17-yl)ethan-1-one
;
_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                111.561(4)
_cell_angle_beta                 96.486(4)
_cell_angle_gamma                97.128(4)
_cell_formula_units_Z            1
_cell_length_a                   6.3144(8)
_cell_length_b                   9.7315(13)
_cell_length_c                   10.5867(14)
_cell_measurement_reflns_used    6602
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.71
_cell_measurement_theta_min      4.20
_cell_volume                     591.41(14)
_computing_cell_refinement       'SAINT (Brucker, 2012)[2]'
_computing_data_collection       'APEX2 (Brucker, 2012)[2]'
_computing_data_reduction        'SAINT (Brucker, 2012)[2]'
_computing_molecular_graphics    'Diamond 4.0[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[1]'
_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 0.977
_diffrn_measured_fraction_theta_max 0.984
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29665
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.592
_diffrn_reflns_theta_min         4.202
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Flack x determined using 1790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         10643
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1444
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0786P)^2^+0.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.985
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                4969
_reflns_number_total             10643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0105_suppl_001.cif
_cod_data_source_block           A
_cod_database_code               8107500
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              86049
_shelx_hkl_checksum              56030