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_4323533
_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 P2 F12 O2 N8 C17 H27'
_chemical_formula_sum            'C17 H27 F12 N8 O2 P2 Re'
_chemical_formula_weight         851.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.022(3)
_cell_length_b                   13.022
_cell_length_c                   17.218(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      22.00
_cell_measurement_theta_min      20.00
_cell_volume                     2919.7(11)
_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      294(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  0.060
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17948
_diffrn_reflns_theta_max         69.73
_diffrn_reflns_theta_min         4.80
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    9.93
_exptl_absorpt_correction_T_max  0.3355
_exptl_absorpt_correction_T_min  0.0666
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00057(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-93 (Sheldrick,1995)'
_refine_ls_goodness_of_fit_all   0.916
_refine_ls_goodness_of_fit_obs   1.027
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_restrained_S_obs      1.027
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_obs          0.0271
_refine_ls_shift/esd_max         0.964
_refine_ls_shift/esd_mean        0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0758
_refine_ls_wR_factor_obs         0.0698
_reflns_number_observed          979
_reflns_number_total             1396
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970067w_1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0483P)^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^)+(0.0483P)^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_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4323533