Oxo Ligand Reactivity in the [ReO2L4]+ Complex of 1-Methylimidazole. Preparation and Crystal Structures of Salts Containing the ReOL43+ Core and Apical CH3O-, BF3O2-, and (CH3O)2PO2- Groups
Suzanne Bélanger; André L. Beauchamp; Inorganic Chemistry 36 (1997) 3640–3647; doi:10.1021/ic970067w

data_4323534
_publ_section_title
;
 Oxo Ligand Reactivity in the [ReO2L4]+ Complex of 1-Methylimidazole.
 Preparation and Crystal Structures of Salts Containing the ReOL43+ Core
 and Apical CH3O-, BF3O2-, and (CH3O)2PO2- Groups
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3640
_journal_page_last               3647
_journal_paper_doi               10.1021/ic970067w
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'Re P3 F12 O5 N8 C25 H38'
_chemical_formula_sum            'C25 H38 F12 N8 O5 P3 Re'
_chemical_formula_weight         1037.75
_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-93 (Sheldrick,1995)'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.83(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.165(4)
_cell_length_b                   13.052(6)
_cell_length_c                   20.931(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      10.50
_cell_measurement_theta_min      10.00
_cell_volume                     3850(2)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       'Theta/2theta scan b/P/b'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Copper K\a'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24362
_diffrn_reflns_theta_max         69.63
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        11.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    7.74
_exptl_absorpt_correction_T_max  0.6768
_exptl_absorpt_correction_T_min  0.4338
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.918
_refine_ls_goodness_of_fit_obs   1.022
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_restrained_S_obs      1.022
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_obs          0.0373
_refine_ls_shift/esd_max         0.561
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0903
_refine_ls_wR_factor_obs         0.0853
_reflns_number_observed          5173
_reflns_number_total             6993
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970067w_2.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] 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^)+(0.0368P)^2^+0.0000P] 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        3849.7(24)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4323534