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_4322467
_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     '[ReO(OSiMe3){H2B(pz)2}2]'
_chemical_formula_sum            'C15 H25 B2 N8 O2 Re Si'
_chemical_formula_weight         585.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.785(2)
_cell_length_b                   17.680(2)
_cell_length_c                   11.971(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      10.2
_cell_volume                     2256.5(6)
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4202
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.466
_exptl_absorpt_correction_T_max  0.9971
_exptl_absorpt_correction_T_min  0.8009
_exptl_absorpt_correction_type   'empirical via\y-scan North et al(1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.961
_refine_ls_goodness_of_fit_obs   0.898
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_restrained_S_obs      0.898
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_obs          0.0257
_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^)+(0.0361P)^2^+6.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_obs         0.0577
_reflns_number_observed          3346
_reflns_number_total             3979
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990229j_2.cif
_cod_data_source_block           C15H25B2N8O2ReSi
_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^)+(0.0361P)^2^+6.2609P] 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^)+(0.0361P)^2^+6.2609P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322467