1-Bromo-1'-(diphenylthiophosphoryl)ferrocene
Štěpnička, Petr; Schulz, Jiří; Císařová, Ivana; Acta Crystallographica Section E 65 (2009) m1210–; doi:10.1107/S1600536809036459

data_2223355
_publ_section_title
;
 1-Bromo-1'-(diphenylthiophosphoryl)ferrocene
;
_journal_coeditor_code           DN2483
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1210
_journal_paper_doi               10.1107/S1600536809036459
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe (C5 H4 Br) (C17 H14 P S)]'
_chemical_formula_moiety         'C22 H18 Br Fe P S'
_chemical_formula_sum            'C22 H18 Br Fe P S'
_chemical_formula_weight         481.15
_chemical_name_systematic
;
1'-(diphenylthiophosphoryl)-1-bromoferrocene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.460(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3590(7)
_cell_length_b                   17.3446(7)
_cell_length_c                   17.0297(9)
_cell_measurement_reflns_used    74781
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     3853.0(3)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \p scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1218
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53227
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.051
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(COLLECT; Nonius, 2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.190
_refine_diff_density_min         -1.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1396
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1118P)^2^+21.2954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2316
_reflns_number_gt                4020
_reflns_number_total             6802
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2483.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               2223355
_cod_database_fobs_code          2223355