Neutral trans-Dioxorhenium(V) Complexes with the Anionic Tetrakis(pyrazolyl)borate Ligand
António Paulo; K. Rajender Reddy; Ângela Domingos; Isabel Santos; Inorganic Chemistry 37 (1998) 6807–6813; doi:10.1021/ic980422y

data_4323244
_publ_section_title
;
 Neutral trans-Dioxorhenium(V) Complexes with the Anionic
 Tetrakis(pyrazolyl)borate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6807
_journal_page_last               6813
_journal_paper_doi               10.1021/ic980422y
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C29 H38 B Cl6 N12 O2 Re'
_chemical_formula_weight         996.42
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.910(10)
_cell_angle_beta                 102.370(10)
_cell_angle_gamma                94.210(10)
_cell_formula_units_Z            2
_cell_length_a                   10.907(2)
_cell_length_b                   11.113(1)
_cell_length_c                   16.922(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      8.7
_cell_volume                     1973.2(5)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'MOLEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johonson, 1976)'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6567
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.531
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       irregular
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_obs          0.0311
_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^)+(0.0413P)^2^+2.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0787
_refine_ls_wR_factor_obs         0.0721
_reflns_number_observed          5555
_reflns_number_total             6199
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980422y_1.cif
_cod_data_source_block           COMPLEX5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.5717P] 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^)+(0.0413P)^2^+2.5717P] 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      'P 1'
_cod_database_code               4323244