Salts of the bis(catecholato)borate anion with rhodium– and iridium–phosphine complex cations
Clegg, William; Elsegood, Mark R.J.; Scott, Andrew J.; Marder, Todd B.; Dai, Chaoyang; Norman, Nicholas C.; Pickett, Nigel L.; Robins, Edward G.; Acta Crystallographica Section C 55 (1999) 733–739; doi:10.1107/S0108270199000323

data_2008477
_publ_section_title
;
 Salts of the bis(catecholato)borate anion with rhodium-- and
 iridium--phosphine complex cations
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              733
_journal_page_last               739
_journal_paper_doi               10.1107/S0108270199000323
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         '[Rh(C3 H9 P)4 ] +, C12 H8 B O4 -'
_chemical_formula_sum            'C24 H44 B O4 P4 Rh'
_chemical_formula_weight         634.19
_chemical_name_systematic
;
 tetrakis(trimethylphosphine)rhodium(I)
 bis(catecholato)borate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.541(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7315(9)
_cell_length_b                   29.559(3)
_cell_length_c                   10.8716(10)
_cell_measurement_reflns_used    8136
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.25
_cell_volume                     3052.6(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18627
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.555
_refine_ls_extinction_coef       0.00087(14)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0293P)^2^+2.4605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                5320
_reflns_number_total             6970
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1074.cif
_cod_data_source_block           4
_cod_original_cell_volume        3052.7(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008477