Redox-active catecholate complexes of rhodium hydrotris(pyrazolyl)borates
Connelly, Neil G.; Emslie, David J. H.; Hayward, Owen D.; Orpen, A. Guy; Quayle, Michael J.; Journal of the Chemical Society, Dalton Transactions  (2001) 875–; doi:10.1039/b010061g

data_7010515
_publ_section_title
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 Redox-active catecholate complexes of rhodium
 hydrotris(pyrazolyl)borates
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_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              875
_journal_paper_doi               10.1039/b010061g
_journal_year                    2001
_chemical_formula_structural     '[Rh(PPh3)(Tp)(O2C6Cl4)]CH2Cl2'
_chemical_formula_sum            'C40 H39 B Cl6 N6 O2 P Rh'
_chemical_formula_weight         993.16
_chemical_name_systematic
; 
? 
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_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.053(4)
_cell_length_b                   14.046(4)
_cell_length_c                   14.439(3)
_cell_measurement_reflns_used    224
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     4269.8(17)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frame'
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26097
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00051(9)
_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   1.115
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0459
_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^)+(0.0252P)^2^+4.2747P] where where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0932
_refine_ls_wR_factor_obs         0.0779
_reflns_number_observed          3421
_reflns_number_total             5068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b010061g.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+4.2747P] where 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^)+(0.0252P)^2^+4.2747P] where where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4269.9(17)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7010515