Synthesis and Characterization of (Tris(3,5-dimethylpyrazolyl)borato)rhodium Alkyl and Vinyl Chloride Complexes
Douglas D. Wick; William D. Jones; Inorganic Chemistry 36 (1997) 2723–2729; doi:10.1021/ic961337y

data_4323472
_publ_contact_author
;
William D. Jones
Department of Chemistry
University of Rochester
Rochester, NY  14627
;
_publ_contact_author_email       ' jones@chem.rochester.edu '
_publ_contact_author_fax         ' 716-473-6889 '
_publ_contact_author_phone       ' 716-275-5493'
_publ_section_title
;
 Synthesis and Characterization of
 (Tris(3,5-dimethylpyrazolyl)borato)rhodium Alkyl and Vinyl Chloride
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2723
_journal_page_last               2729
_journal_paper_doi               10.1021/ic961337y
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H31 B Cl2 N6 P Rh'
_chemical_formula_weight         547.08
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 111.6360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9384(6)
_cell_length_b                   17.3111(9)
_cell_length_c                   13.5132(7)
_cell_measurement_reflns_used    7097
_cell_measurement_temperature    223
_cell_measurement_theta_max      46.5
_cell_measurement_theta_min      4
_cell_volume                     2378.5(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9264
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  .93
_exptl_absorpt_correction_T_min  .78
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .22
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0238
_refine_ls_shift/esd_max         -0.045
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+1.5986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0581
_refine_ls_wR_factor_obs         0.0553
_reflns_number_observed          2990
_reflns_number_total             3398
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961337y_3.cif
_cod_data_source_block           RhTp'(Cl)2(PMe3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+1.5986P] 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^)+(0.0276P)^2^+1.5986P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323472