16α,17α-Epoxy-5α-hydroxy-6β-nitrooxy-20-oxopregnan-3β-yl acetate
Pinto, R. M. A.; Matos Beja, A.; Salvador, J. A. R.; Paixão, J. A.; Acta Crystallographica Section E 65 (2009) o1271–o1272; doi:10.1107/S1600536809016997

data_2221931
_publ_section_title
;
 16\a,17\a-Epoxy-5\a-hydroxy-6\b-nitrooxy-20-oxopregnan-3\b-yl acetate
;
_journal_coeditor_code           BT2943
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1271
_journal_page_last               o1272
_journal_paper_doi               10.1107/S1600536809016997
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C23 H33 N O8'
_chemical_formula_moiety         'C23 H33 N O8'
_chemical_formula_sum            'C23 H33 N O8'
_chemical_formula_weight         451.50
_chemical_melting_point          455
_chemical_name_systematic
;
16\a,17\a-Epoxy-5\a-hydroxy-6\b-nitrooxy-20-oxopregnan-3\b-yl acetate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                77.2135(15)
_cell_angle_beta                 73.2087(14)
_cell_angle_gamma                64.3465(14)
_cell_formula_units_Z            2
_cell_length_a                   10.9740(3)
_cell_length_b                   11.0721(3)
_cell_length_c                   11.1686(3)
_cell_measurement_reflns_used    9093
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.3318
_cell_measurement_theta_min      2.2901
_cell_volume                     1163.81(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24934
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated pyramid'
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.1756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                4806
_reflns_number_total             5770
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2943.cif
_cod_data_source_block           I
_cod_database_code               2221931
_cod_database_fobs_code          2221931