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_4323246
_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            'C18 H30 B N8 O2 P2 Re'
_chemical_formula_weight         649.45
_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                   18.422(2)
_cell_length_b                   11.850(1)
_cell_length_c                   11.434(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      8.3
_cell_volume                     2496.1(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 (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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2988
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        3.3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.028
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00229(14)
_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   1.071
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_obs          0.0288
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+5.8043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0680
_refine_ls_wR_factor_obs         0.0596
_reflns_number_observed          1931
_reflns_number_total             2306
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980422y_3.cif
_cod_data_source_block           COMPLEX10
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+5.8043P] 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^)+(0.0290P)^2^+5.8043P] 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_database_code               4323246