(1<i>S</i>,3<i>R</i>)-<i>N</i>-{(3<i>S</i>,10<i>S</i>,12<i>S</i>,13<i>R</i>,17<i>R</i>)-12-Hydroxy-17-[(<i>R</i>)-5-hydroxypentan-2-yl]-10,13-dimethylhexadecahydro-1<i>H</i>-cyclopenta[<i>a</i>]phenanthren-3-yl}adamantane-1-carboxamide 0.25-hydrate
Campos Fernandez, Cristian; Procupez-Schtirbu, R.; Soto-Tellini, V. H.; Salazar, J. C.; Jancik, Vojtech; IUCrData 7 (2022) x220947–; doi:10.1107/S2414314622009476

data_1567766
_publ_section_title
;
 (1<i>S</i>,3<i>R</i>)-<i>N</i>-{(3<i>S</i>,10<i>S</i>,12<i>S</i>,13<i>R</i>,17<i>R</i>)-12-Hydroxy-17-[(<i>R</i>)-5-hydroxypentan-2-yl]-10,13-dimethylhexadecahydro-1<i>H</i>-cyclopenta[<i>a</i>]phenanthren-3-yl}adamantane-1-carboxamide
 0.25-hydrate
;
_journal_coeditor_code           BT4124
_journal_issue                   10
_journal_name_full               IUCrData
_journal_page_first              x220947
_journal_paper_doi               10.1107/S2414314622009476
_journal_volume                  7
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C35 H57 N O3, 0.25H2 O'
_chemical_formula_moiety         'C35 H57 N O3, 0.25(H2 O)'
_chemical_formula_sum            'C35 H57.5 N O3.25'
_chemical_formula_weight         544.32
_chemical_name_systematic
'(1<i>S</i>,3<i>R</i>)-<i>N</i>-{(3<i>S</i>,10<i>S</i>,12<i>S</i>,13<i>R</i>,17<i>R</i>)-12-Hydroxy-17-[(<i>R</i>)-5-hydroxypentan-2-yl]-10,13-dimethylhexadecahydro-1<i>H</i>-cyclopenta[<i>a</i>]phenanthren-3-yl}adamantane-1-carboxamide 0.25-hydrate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                116.2071(14)
_cell_angle_beta                 91.0059(15)
_cell_angle_gamma                100.4537(15)
_cell_formula_units_Z            4
_cell_length_a                   11.8289(6)
_cell_length_b                   16.7287(8)
_cell_length_c                   17.7234(9)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.60
_cell_volume                     3075.4(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008b)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008b)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22679
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.462
_diffrn_source
'sealed tube, Siemens KFFMO2K-90 with curved graphite'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.74521
_exptl_absorpt_correction_T_min  0.69132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             1202
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.248
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 7166 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1612
_refine_ls_number_reflns         22679
_refine_ls_number_restraints     999
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0371P)^2^+2.3114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                18020
_reflns_number_total             22679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4124.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C35 H57.50 N O3.25'
_cod_database_code               1567766
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.985
_shelx_hkl_checksum              92458
_shelx_res_checksum              28681