16α-Chloro-16β-cyano-3-methoxy-14,17α-ethenoestra-1,3,5(10)-trien-17β-yl Acetate
Bull, James R.; de Koning, Pieter D.; Acta Crystallographica Section C 54 (1998) 1281–1282; doi:10.1107/S0108270198000584

data_2007672
_publ_section_title
;
 16\a-Chloro-16\b-cyano-3-methoxy-14,17\a-ethenoestra-1,3,5(10)-trien-17\b-yl
 Acetate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1281
_journal_page_last               1282
_journal_paper_doi               10.1107/S0108270198000584
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C24 H26 Cl N O3'
_chemical_formula_sum            'C24 H26 Cl N O3'
_chemical_formula_weight         411.91
_chemical_melting_point          456.6(15)
_chemical_name_systematic
;
16\a-Chloro-16\b-cyano-3-methoxy-14,17\a-ethenoestra-1,3,5(10)-
 trien-17\b-yl Acetate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 98.503(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.638(3)
_cell_length_b                   8.650(2)
_cell_length_c                   15.778(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      16
_cell_volume                     2110.8(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software'
_computing_molecular_graphics    'ZORTEP (Zsolnai & Pritzkow, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    6.8741
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4140
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.285
_refine_ls_abs_structure_details
;
 assigned from the estrone precursor
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.972
_refine_ls_goodness_of_fit_obs   1.299
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_restrained_S_obs      1.299
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_obs          .064
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.161
_refine_ls_wR_factor_obs         .1510
_reflns_number_observed          2218
_reflns_number_total             3987
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sx1056.cif
_cod_data_source_block           bull
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '182-185\%C' was changed to
'456.6(15)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '182-185\%C' was changed to
'456.6(15)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.1P)^2^] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2110.8(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C24 H26 Cl1 N1 O3'
_cod_database_code               2007672