[1,1'-Bis(diphenylphosphanyl)cobaltocenium]carbonylchloridohydrido(triphenylphosphane)ruthenium(II) hexafluoridophosphate dichloromethane disolvate
Hou, Jian-Guo; Acta Crystallographica Section E 67 (2011) m1671–m1672; doi:10.1107/S1600536811044035

data_2232772
_publ_section_title
;
 [1,1'-Bis(diphenylphosphanyl)cobaltocenium]carbonylchloridohydrido(triphenylphosphane)ruthenium(II)
 hexafluoridophosphate dichloromethane disolvate
;
_journal_coeditor_code           HY2477
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1671
_journal_page_last               m1672
_journal_paper_doi               10.1107/S1600536811044035
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Co Ru (C17 H14 P)2 Cl H (C18 H15 P) (C O)] P F6, 2C H2 Cl2'
_chemical_formula_moiety
'C53 H44 Cl Co O P3 Ru +, F6 P -, 2(C H2 Cl2)'
_chemical_formula_sum            'C55 H48 Cl5 Co F6 O P4 Ru'
_chemical_formula_weight         1300.06
_chemical_name_systematic
;
[1,1'-Bis(diphenylphosphanyl)cobaltocenium]carbonylchloridohydrido
(triphenylphosphane)ruthenium(II) hexafluoridophosphate dichloromethane
disolvate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   22.5676(19)
_cell_length_b                   22.0330(18)
_cell_length_c                   11.0614(9)
_cell_measurement_reflns_used    6748
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.25
_cell_volume                     5500.1(8)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63147
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.8258
_exptl_absorpt_correction_T_min  0.7545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.366
_refine_ls_abs_structure_details 'Flack (1983), 6103 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.002(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         13058
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                11469
_reflns_number_total             13058
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2477.cif
_cod_data_source_block           I
_cod_database_code               2232772
_cod_database_fobs_code          2232772