Crystal structure of isotibolone: a major degradation product of tibolone
Gomez, Ariel; Antonio, Selma Gutierrez; Barros de Araujo, Gabriel Lima; Ferreira, Fabio Furlan; Paiva-Santos, Carlos Oliveira; CrystEngComm 14 (2012) 2826–; doi:10.1039/c2ce06504e

data_7207593
_publ_section_title
;
 Crystal structure of isotibolone: a major degradation product of tibolone
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2826
_journal_paper_doi               10.1039/c2ce06504e
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C21 H28 O2'
_chemical_formula_sum            'C21 H28 O2'
_chemical_formula_weight         312.446
_chemical_name_common
;(7alpha,17beta)-17-ethynyl-17-hydroxy-7-methylestr-4(5)en-3-
one
;
_chemical_name_systematic
;
(7alpha,17beta)-17-ethynyl-17-hydroxy-7-methylestr-4(5)en-3-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'TOPAS ACADEMIC 4.1 + PLATON'
_audit_update_record
;
2012-01-11 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 76.4302(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.80704(7)
_cell_length_b                   20.73858(18)
_cell_length_c                   6.44900(6)
_cell_measurement_temperature    298(2)
_cell_volume                     884.981(15)
_computing_cell_refinement       'Topas Academic v.4.1'
_computing_data_collection       'Win X-POW'
_computing_data_reduction        'Topas Academic v.4.1'
_computing_molecular_graphics    'Mercury 2.4'
_computing_publication_material  'TOPAS ACADEMIC 4.1'
_computing_structure_refinement  'TOPAS ACADEMIC 4.1'
_computing_structure_solution    'ab initio algorithm'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Stoe STADI-P powder diffractometer'
_diffrn_radiation_monochromator  'curved Ge(111) monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.54056
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
TOPAS:
capillary_diameter_mm 0.28
capillary_u_cm_inv !absc 229 '(in 1_on_cm)
capillary_parallel_beam
;
_exptl_crystal_density_diffrn    1.1725
_exptl_crystal_density_meas      1.1467
_exptl_crystal_density_method    'picnometric measurement'
_exptl_crystal_F_000             340
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  white
_pd_meas_number_of_points        7600
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        78
_pd_proc_2theta_range_min        2
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  '20-term Chebyschev polynomial'
_pd_proc_ls_pref_orient_corr     '4 terms spherical harmonics'
_pd_proc_ls_profile_function     'Fundamental parameters approach'
_pd_proc_ls_prof_R_factor        0.02713
_pd_proc_ls_prof_wR_expected     0.01928
_pd_proc_ls_prof_wR_factor       0.03557
_pd_proc_number_of_points        7600
_pd_spec_mounting                'special glass capillary'
_pd_spec_mount_mode              transmission
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.845
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     108
_refine_ls_number_restraints     68
_refine_ls_R_Fsqd_factor         0.00847
_refine_ls_R_I_factor            0.01984
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0001
_refine_ls_weighting_details     chi**2=(1/sum(wmYo,m)*[sum(wm(Yo,m-Yc,m)**2)]
_refine_ls_weighting_scheme      sigma
_reflns_d_resolution_high        10.3692
_reflns_d_resolution_low         1.2178
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              4
_reflns_limit_l_min              -4
_reflns_number_total             394
_cod_data_source_file            c2ce06504e.txt
_cod_data_source_block           Isotibolone
_cod_original_cell_volume        884.980(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7207593