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_4321653
_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)(Bpz4)(dmpe)]Cl'
_chemical_formula_sum            'C22 H39 B Cl3 N8 O2 P2 Re Si'
_chemical_formula_weight         841.00
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   11.311(2)
_cell_length_b                   19.135(2)
_cell_length_c                   15.443(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      7.9
_cell_volume                     3342.4(8)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3063
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.041
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   'empirical via \y-scan North et al (1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plates
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.047
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_obs          0.0460
_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^)+(0.0569P)^2^+24.2666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1242
_refine_ls_wR_factor_obs         0.1022
_reflns_number_observed          2496
_reflns_number_total             3063
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000481n_1.cif
_cod_data_source_block           C22H39BCl3N8O2P2ReSi
_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^)+(0.0569P)^2^+24.2666P] 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^)+(0.0569P)^2^+24.2666P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P b a 21'
_cod_database_code               4321653