Cationic Re(V) Oxo Complexes with Poly(pyrazolyl)borates: Synthesis, Characterization, and Stability
António Paulo; Ângela Domingos; Raquel Garcia; Isabel Santos; Inorganic Chemistry 39 (2000) 5669–5674; doi:10.1021/ic000481n

data_4321655
_publ_section_title
;
 Cationic Re(V) Oxo Complexes with Poly(pyrazolyl)borates: Synthesis,
 Characterization, and Stability
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5669
_journal_page_last               5674
_journal_paper_doi               10.1021/ic000481n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[ReO(OSiMe3)(Cl)(Bpz4)(1-Meimz)](7)'
_chemical_formula_sum            'C19 H27 B Cl N10 O2 Re Si'
_chemical_formula_weight         688.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.971(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.356(2)
_cell_length_b                   20.384(3)
_cell_length_c                   17.360(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5535.8(15)
_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)
_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\qscans
_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  0.0841
_diffrn_reflns_av_sigmaI/netI    0.1714
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10077
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.565
_exptl_absorpt_correction_T_max  0.9089
_exptl_absorpt_correction_T_min  0.8083
_exptl_absorpt_correction_type   'empirical via \y-scan North et al (1968)'
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.201
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         7776
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.269
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.2158
_refine_ls_R_factor_obs          0.0852
_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^)+(0.0179P)^2^+26.9673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1594
_refine_ls_wR_factor_obs         0.0972
_reflns_number_observed          4397
_reflns_number_total             9713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000481n_3.cif
_cod_data_source_block           C19H27BClN10O2ReSi
_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^)+(0.0179P)^2^+26.9673P] 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^)+(0.0179P)^2^+26.9673P] 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        5535.8(14)
_cod_database_code               4321655