Crystal structure of (20<i>S</i>)-21-[4-(2-hydroxypropan-2-yl)-1<i>H</i>-1,2,3-triazol-4-yl]-20-(4-methylpentyl)-5-pregnen-3β-ol with an unknown solvate
Santalla, Hugo; Argibay, Saray; Acta Crystallographica Section E 74 (2018) 465–468; doi:10.1107/S2056989018003286

data_2242410
_publ_section_title
;
 Crystal structure of
 (20<i>S</i>)-21-[4-(2-hydroxypropan-2-yl)-1<i>H</i>-1,2,3-triazol-4-yl]-20-(4-methylpentyl)-5-pregnen-3\b-ol
 with an unknown solvate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              465
_journal_page_last               468
_journal_paper_doi               10.1107/S2056989018003286
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C32 H53 N3 O'
_chemical_formula_moiety         'C32 H53 N3 O2'
_chemical_formula_sum            'C32 H53 N3 O2'
_chemical_formula_weight         511.77
_chemical_name_systematic
(20<i>S</i>)-21-[4-(2-Hydroxypropan-2-yl)-1<i>H</i>-1,2,3-triazol-4-yl]-20-(4-methylpentyl)-5-pregnen-3\b-ol
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 97.452(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1130(15)
_cell_length_b                   10.3898(7)
_cell_length_c                   15.5934(12)
_cell_measurement_reflns_used    9096
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.50
_cell_volume                     3231.0(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and Mercury (Macrae <i>et
al.</i>,  2008)
;
_computing_publication_material
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b), PLATON (Spek, 2009)
and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            85013
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         2.504
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.235
_platon_squeeze_details
;
TITL II
CELL   20.1130   10.3898   15.5934     90.00     97.45     90.00
SPGR C2
Q101 0.519 0.254 0.097 !       5.87 eA-3
C102 0.527 0.162 0.034 !       5.01 eA-3
C103 0.011 0.459 0.049 !       4.05 eA-3
C104 0.438 0.038 0.829 !       3.31 eA-3
C105 0.537 0.020 0.102 !       2.84 eA-3
C106 0.500 0.250 0.000 !       1.88 eA-3
C107 0.444 0.092 0.006 !       0.86 eA-3
;
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.307
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3430 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         8040
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.6246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                7629
_reflns_number_total             8040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2005sup1.cif
_cod_data_source_block           2
_cod_database_code               2242410
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              32713
_shelx_res_checksum              31763
_shelx_fab_checksum              46854