Dichlorotris(triphenylphosphine)ruthenium(II) dichloromethane hemisolvate
Cowley, Andrew R.; Dilworth, Jonathan R.; Maresca von Beckh W., Carlo A.; Acta Crystallographica Section E 61 (2005) m1237–m1239; doi:10.1107/S1600536805016272

data_2205953
_publ_section_title
;
 Dichlorotris(triphenylphosphine)ruthenium(II) dichloromethane
 hemisolvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1237
_journal_page_last               m1239
_journal_paper_doi               10.1107/S1600536805016272
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ru Cl2 (C18 H15 P)3] , 0.5C H2 Cl2'
_chemical_formula_moiety         'C54 H45 Cl2 P3 Ru , 0.5C H2 Cl2'
_chemical_formula_sum            'C54.5 H46 Cl3 P3 Ru'
_chemical_formula_weight         1001.31
_chemical_name_systematic
;
Dichlorotris(triphenylphosphine)ruthenium(II) dichloromethane hemisolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.5681(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2083(2)
_cell_length_b                   12.84460(10)
_cell_length_c                   33.9272(5)
_cell_measurement_reflns_used    17441
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      5.0
_cell_volume                     9226.57(18)
_computing_cell_refinement       'DENZO and SCALEPACK'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            17441
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         5.107
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(DENZO and SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple-brown
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.76
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6083
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994; Prince, 1982).
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~
are the Chebychev coefficients 0.437 0.688E-01 0.160 and x = Fcalc/Fmax.
Method, part 2, Robust Weighting (Prince, 1982). W =
[weight]*[1-(deltaF/6*sigmaF)^2^]^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0777
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                6083
_reflns_number_total             10441
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hb6207.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C54.50 H46 Cl3 P3 Ru1'
_cod_database_code               2205953