Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-κ<i>S</i>)(triphenylphosphane-κ<i>P</i>)osmium(IV): a monoclinic polymorph
Zeleny, Paulina; Arroyo, Maribel; Meléndez, Lidia; Bernès, Sylvain; IUCrData 4 (2019) x191622–; doi:10.1107/S2414314619016225

data_1556895
_publ_section_title
;
 Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-\k<i>S</i>)(triphenylphosphane-\k<i>P</i>)osmium(IV):
 a monoclinic polymorph
;
_journal_coeditor_code           ZL4036
_journal_issue                   12
_journal_name_full               IUCrData
_journal_page_first              x191622
_journal_paper_doi               10.1107/S2414314619016225
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          '[Os (C6 H F4 S)4 (C18 H15 P)]'
_chemical_formula_moiety         'C42 H19 F16 Os P S4'
_chemical_formula_sum            'C42 H19 F16 Os P S4'
_chemical_formula_weight         1176.98
_chemical_name_systematic
Tetrakis(2,3,5,6-tetrafluorobenzenethiolato-\k<i>S</i>)(triphenylphosphane-\k<i>P</i>)osmium(IV)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.991(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4008(5)
_cell_length_b                   13.8892(7)
_cell_length_c                   25.2321(11)
_cell_measurement_reflns_used    22104
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      23.45
_cell_measurement_theta_min      2.03
_cell_volume                     4266.2(3)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2018)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2018)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2018)
;
_computing_molecular_graphics
;
XP in SHELXTL-Plus (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2018)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector                 'Reverse-biased silicon diode array'
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Eulerian four-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.1858
_diffrn_reflns_av_unetI/netI     0.1192
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            93107
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         20.504
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_current           0.55
_diffrn_source_power             0.03575
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(X-AREA; Stoe & Cie, 2018)
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.710
_refine_diff_density_min         -1.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                4264
_reflns_number_total             8692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl4036sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556895
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              99090
_shelx_res_checksum              99106
_cod_database_fobs_code 1556895