Coordination of Tetrakis(pyrazolyl)borate in Rhenium Complexes Containing the [ReVO]3+ Core
António Paulo; Ângela Domingos; Isabel Santos; Inorganic Chemistry 35 (1996) 1798–1807; doi:10.1021/ic950972l

data_4324057
_publ_section_title
;
 Coordination of Tetrakis(pyrazolyl)borate in Rhenium Complexes Containing
 the [ReVO]3+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1798
_journal_page_last               1807
_journal_paper_doi               10.1021/ic950972l
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C31 H32 B2 Cl2 N20 O3 Re2'
_chemical_formula_weight         1197.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.51(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.086(2)
_cell_length_b                   15.269(1)
_cell_length_c                   12.133(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.90
_cell_measurement_theta_min      10.06
_cell_volume                     2049.9(4)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'MOLEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976) '
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer '
_diffrn_measurement_method       '\w/2\q scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8272
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.091
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_description       'hexagonal plate '
_exptl_crystal_F_000             1148
_refine_diff_density_max         1.172
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_obs          0.0299
_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^)+(0.0544P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0843
_refine_ls_wR_factor_obs         0.0741
_reflns_number_observed          6717
_reflns_number_total             7203
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950972l_3.cif
_cod_data_source_block           C30H30B2N20O3Re2.CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+0.5891P] 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^)+(0.0544P)^2^+0.5891P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C31 H32 B2 N20 O3 Re2 Cl2'
_cod_database_code               4324057