Rhenium(V) Dioxo Complexes with Dihydrobis(pyrazolyl)borates: Synthesis and Reactivity toward Electrophilic Substrates
K. Rajender Reddy; Ângela Domingos; António Paulo; Isabel Santos; Inorganic Chemistry 38 (1999) 4278–4282; doi:10.1021/ic990229j

data_4322466
_publ_section_title
;
 Rhenium(V) Dioxo Complexes with Dihydrobis(pyrazolyl)borates: Synthesis
 and Reactivity toward Electrophilic Substrates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4278
_journal_page_last               4282
_journal_paper_doi               10.1021/ic990229j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_structural     '[ReO2(py)4][ReO2{H2B(pz)2}2].CH2Cl2'
_chemical_formula_sum            'C17 H20 B Cl2 N6 O2 Re'
_chemical_formula_weight         608.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                89.030(10)
_cell_angle_beta                 82.410(10)
_cell_angle_gamma                72.750(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4190(10)
_cell_length_b                   9.5840(10)
_cell_length_c                   12.6520(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      8.7
_cell_volume                     1080.89(19)
_computing_cell_refinement       'CAD4 software (Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software (Enraf-Nonius,1989)'
_computing_data_reduction        'process-MOLEN (Fair,1990)'
_computing_molecular_graphics    'ORTEP (Johnson,1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscan
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4033
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.894
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.4670
_exptl_absorpt_correction_type   'empirical via\y-scan North et al (1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3782
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.180
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_obs          0.0313
_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^)+(0.0333P)^2^+2.4412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0798
_refine_ls_wR_factor_obs         0.0674
_reflns_number_observed          2850
_reflns_number_total             3783
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990229j_1.cif
_cod_data_source_block           C17H20BCl2N6O2Re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+2.4412P] 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^)+(0.0333P)^2^+2.4412P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1080.9(2)
_cod_database_code               4322466