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_2008476
_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
'[RhClH(C26 H48 P2 )2 ] +, C12 H8 B O4 -, 4C H2 Cl2'
_chemical_formula_sum            'C68 H113 B Cl9 O4 P4 Rh'
_chemical_formula_weight         1551.23
_chemical_name_systematic
;
 trans-chlorohydridobis(1,2-bis(dicyclohexylphosphino)ethane)rhodium(III)
 bis(catecholato)borate dichloromethane tetrasolvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   13.9320(8)
_cell_length_b                   21.2938(10)
_cell_length_c                   25.5613(14)
_cell_measurement_reflns_used    14978
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      1.66
_cell_volume                     7583.1(7)
_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 0.970
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27335
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.082
_refine_diff_density_min         -2.127
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         14673
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+48.7217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                13157
_reflns_number_total             14673
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1074.cif
_cod_data_source_block           3
_cod_database_code               2008476