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_2008474
_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         '[IrClH(C6 H15 P)4] +, C12 H8 B O4 -'
_chemical_formula_sum            'C36 H69 B Cl Ir O4 P4'
_chemical_formula_weight         928.25
_chemical_name_systematic
;
 cis-chlorohydridotetrakis(triethylphosphine)iridium(III)
 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                 102.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.276(3)
_cell_length_b                   15.290(3)
_cell_length_c                   19.807(4)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      11.64
_cell_volume                     4223.3(15)
_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, 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe-Bruker diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8170
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  0.347
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 1994)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.130
_refine_ls_extinction_coef       0.00010(9)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.8148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                5755
_reflns_number_total             7421
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln1074.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008474