Chloro-<i>cis</i>-dihydro-<i>mer</i>-tris(triphenylphosphine)rhodium(III) dichloromethane hemisolvate
Clegg, William; Elsegood, Mark R. J.; Norman, Nicholas C.; Pickett, Nigel L.; Acta Crystallographica Section E 58 (2002) m406–m407; doi:10.1107/S1600536802012266

data_2201276
_publ_section_title
;
 Chloro-<i>cis</i>-dihydro-<i>mer</i>-tris(triphenylphosphine)rhodium(III)
 dichloromethane hemisolvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m406
_journal_page_last               m407
_journal_paper_doi               10.1107/S1600536802012266
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Rh Cl H2 (C18 H15 P)3], 0.5C H2 Cl2'
_chemical_formula_moiety         'C54 H47 Cl P3 Rh , 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H48 Cl2 P3 Rh'
_chemical_formula_weight         969.6
_chemical_name_systematic
;
Chloro-cis-dihydro-mer-tris(triphenylphosphine)rhodium(III) dichloromethane
hemisolvate
;
_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                83.30(5)
_cell_angle_beta                 83.42(4)
_cell_angle_gamma                76.64(4)
_cell_formula_units_Z            2
_cell_length_a                   9.390(5)
_cell_length_b                   12.581(6)
_cell_length_c                   20.096(10)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.2
_cell_volume                     2285(2)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Stoe--Siemens
_diffrn_measurement_method       \w/\q
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6142
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.675
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0655P)^2^+1.2789P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                4522
_reflns_number_total             5972
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6164.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C54.50 H48 Cl2 P3 Rh'
_cod_database_code               2201276
_cod_database_fobs_code          2201276