Crystal structure of [1,2-bis(diphenylphosphanyl)benzene]heptacarbonyldi-μ-hydrido-(μ~3~-2,4,6-trimethylphenylphosphinidene)-<i>triangulo</i>-triruthenium
Kakizawa, Taeko; Acta Crystallographica Section E 73 (2017) 945–948; doi:10.1107/S2056989017007770

data_2242196
_publ_section_title
;
 Crystal structure of
 [1,2-bis(diphenylphosphanyl)benzene]heptacarbonyldi-\m-hydrido-(\m~3~-2,4,6-trimethylphenylphosphinidene)-<i>triangulo</i>-triruthenium
;
_journal_coeditor_code           IS5476
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              945
_journal_page_last               948
_journal_paper_doi               10.1107/S2056989017007770
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ru3 (C30 H24 P2) (C9 H11 P) (C O)7 H2]'
_chemical_formula_moiety         'C46 H37 O7 P3 Ru3'
_chemical_formula_sum            'C46 H37 O7 P3 Ru3'
_chemical_formula_weight         1097.88
_chemical_name_systematic
'[1,2-Bis(diphenylphosphanyl)benzene]heptacarbonyldi-\m-hydrido-(\m~3~-2,4,6-trimethylphenylphosphinidene)-<i>triangulo</i>-triruthenium'
_space_group_IT_number           2
_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           SHELXL-97
_cell_angle_alpha                114.1719(11)
_cell_angle_beta                 90.2641(14)
_cell_angle_gamma                92.5256(13)
_cell_formula_units_Z            4
_cell_length_a                   10.9732(2)
_cell_length_b                   19.4127(3)
_cell_length_c                   22.1186(2)
_cell_measurement_reflns_used    17326
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.85
_cell_measurement_theta_min      3.74
_cell_volume                     4293.07(12)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation & Rigaku, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30808
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.7946
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.398
_refine_diff_density_min         -1.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         14332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+58.9367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1461
_reflns_number_gt                12888
_reflns_number_total             14332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            is5476sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4293.07(11)
_cod_database_code               2242196
_cod_database_fobs_code 2242196