3-Methoxy-1'-phenyl-4'β,5-dihydro-1<i>H</i>-pyrazolo[4',3':16,17]estra-1,3,5(10)-triene
König, Verena; Schneider, Thomas R.; Frank, Eva; Aukszi, Beatrix; Schneider, Gyula; János Wölfling; Acta Crystallographica Section E 58 (2002) o810–o811; doi:10.1107/S160053680201125X

data_2201700
_publ_section_title
3-Methoxy-1'-phenyl-4'\b,5-dihydro-1<i>H</i>-pyrazolo[4',3':16,17]estra-1,3,5(10)-triene
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o810
_journal_page_last               o811
_journal_paper_doi               10.1107/S160053680201125X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C26 H30 N2 O'
_chemical_formula_moiety         'C26 H30 N2 O'
_chemical_formula_sum            'C26 H30 N2 O'
_chemical_formula_weight         386.52
_chemical_melting_point          .451E-305
_chemical_name_common
;
3-methoxy-1'-phenyl-4'\b,5-dihydro-1H-pyrazolo
[4',3':16,17]estra-1,3,5(10)-triene
;
_chemical_name_systematic
;
3-methoxy-1'-phenyl-4'\b,5-dihydro-1H-pyrazolo
[4',3':16,17]estra-1,3,5(10)-triene
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1200(10)
_cell_length_b                   8.9500(10)
_cell_length_c                   37.622(4)
_cell_measurement_reflns_used    3250
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      2.2
_cell_volume                     2060.7(5)
_computing_cell_refinement       'SAINT (Bruker 1997b)'
_computing_data_collection       'SMART (Siemens 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type
'locally modified Stoe-Siemens-Huber four-circles'
_diffrn_measurement_method       '\f and \w'
_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  0.047
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23229
_diffrn_reflns_theta_full        24.8
_diffrn_reflns_theta_max         24.7
_diffrn_reflns_theta_min         2.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.13
_refine_diff_density_min         -0.16
_refine_ls_abs_structure_details
;Flack (1983); Friedel pairs were merged due to the lack of anomalous
 scatterers
;
_refine_ls_abs_structure_Flack   -1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.038
_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^)+(0.0444P)^2^+0.5351P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                1669
_reflns_number_total             1939
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ya6104.cif
_cod_data_source_block           I
_cod_database_code               2201700
_cod_database_fobs_code          2201700