Synthesis and Characterization of Rhodium(I) Boryl and Rhodium(III) Tris(Boryl) Compounds: Molecular Structures of [(PMe3)4Rh(B(cat))] andfac-[(PMe3)3Rh(B(cat))3] (cat = 1,2-O2C6H4)
Chaoyang Dai; Graham Stringer; Todd B. Marder; Andrew J. Scott; William Clegg; Nicholas C. Norman; Inorganic Chemistry 36 (1997) 272–273; doi:10.1021/ic9611047

data_4323304
_publ_section_title
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 Synthesis and Characterization of Rhodium(I) Boryl and Rhodium(III)
 Tris(Boryl) Compounds: Molecular Structures of [(PMe3)4Rh(B(cat))]
 andfac-[(PMe3)3Rh(B(cat))3] (cat = 1,2-O2C6H4)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              272
_journal_page_last               273
_journal_paper_doi               10.1021/ic9611047
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H40 B O2 P4 Rh'
_chemical_formula_weight         526.10
_chemical_name_systematic
;
 ?
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.728(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7763(12)
_cell_length_b                   9.8236(7)
_cell_length_c                   16.3714(12)
_cell_measurement_reflns_used    11720
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.42
_cell_volume                     2621.0(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens 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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14698
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       Block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.144
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_restrained_S_obs      1.144
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_obs          0.0278
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.0805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0746
_refine_ls_wR_factor_obs         0.0694
_reflns_number_observed          4901
_reflns_number_total             5342
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9611047_1.cif
_cod_data_source_block           tbm13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.0805P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.0805P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4323304