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_4321654
_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(OSiMe)3(Cl)(Bpz4)(4-NMe2py)](6)'
_chemical_formula_sum            'C26 H39 B Cl N10 O3 Re Si'
_chemical_formula_weight         800.22
_chemical_name_systematic
; 
 ? 
;
_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                70.454(7)
_cell_angle_beta                 77.935(9)
_cell_angle_gamma                77.129(8)
_cell_formula_units_Z            2
_cell_length_a                   8.7179(11)
_cell_length_b                   12.5724(8)
_cell_length_c                   17.750(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      8.0
_cell_volume                     1768.1(3)
_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\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  0.0139
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7000
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.587
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   'empirical via \y-scan North et al. (1968)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.089
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.189
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.034
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.9978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1197
_refine_ls_wR_factor_obs         0.1011
_reflns_number_observed          5656
_reflns_number_total             6767
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000481n_2.cif
_cod_data_source_block           C26H39BClN10O3ReSi
_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^)+(0.0649P)^2^+0.9978P] 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^)+(0.0649P)^2^+0.9978P] 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               4321654