Chelation Processes to an Oxorhenium(V) Center by N,N,N,O-Tetradentate and N,N,O-Tridentate Ligands As Verified by Structural and Mechanistic Studies of Intermediate Species
J. Mattheus Botha; Keisuke Umakoshi; Yoichi Sasaki; Gert J. Lamprecht; Inorganic Chemistry 37 (1998) 1609–1615; doi:10.1021/ic971477n

data_4322737
_publ_contact_author
;    Dr. Keisuke Umakoshi
    Division of Chemistry
    Graduate School of Science
    Hokkaido University
    Kita-ku, Sapporo 060
    Japan
;
_publ_contact_author_email       umakoshi@science.hokudai.ac.jp
_publ_contact_author_fax         +81-11-706-3447
_publ_contact_author_phone       +81-11-706-3818
_publ_section_title
;
 Chelation Processes to an Oxorhenium(V) Center by N,N,N,O-Tetradentate
 and N,N,O-Tridentate Ligands As Verified by Structural and Mechanistic
 Studies of Intermediate Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1609
_journal_page_last               1615
_journal_paper_doi               10.1021/ic971477n
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C27 H27.5 Cl F6 N2.5 O2 P2 Re'
_chemical_formula_weight         816.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_type_scat_source           'International Tables (1974)'
_cell_angle_alpha                90.0
_cell_angle_beta                 93.40(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   19.758(6)
_cell_length_b                   9.463(3)
_cell_length_c                   16.297(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    203
_cell_measurement_theta_max      15.90
_cell_measurement_theta_min      10.12
_cell_volume                     3041.7(15)
_computing_cell_refinement       'MXC(MAC Science)'
_computing_data_collection       'MXC(MAC Science)'
_computing_data_reduction        Crystan
_computing_molecular_graphics    Crystan
_computing_publication_material  Crystan
_computing_structure_refinement  Crystan
_computing_structure_solution    SIR92
_diffrn_measurement_device       'Mac Science MXC18'
_diffrn_measurement_method       '\w/2\q scans'
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_diffrn_orient_matrix_UB_12      0.05439
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_diffrn_orient_matrix_UB_21      -0.02742
_diffrn_orient_matrix_UB_22      -0.08847
_diffrn_orient_matrix_UB_23      -0.00674
_diffrn_orient_matrix_UB_31      0.00752
_diffrn_orient_matrix_UB_32      -0.01962
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_diffrn_radiation_type           'Mo K-alpha'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6060
_diffrn_reflns_theta_max         24.23
_diffrn_standards_decay_%        4.745
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.3066
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
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_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.3Ueq(C)'
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_refine_ls_R_factor_obs          0.059
_refine_ls_shift/esd_max         0.0488
_refine_ls_shift/esd_mean        0.0072
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.001F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.069
_reflns_number_observed          3064
_reflns_number_total             4579
_reflns_observed_criterion       I_>_3.00_sigma(I)
_cod_data_source_file            ic971477n_2.cif
_cod_data_source_block           IC971477N-9-a-0/ReOCl(PPh3)(mpenO)(PF6)
_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 'w = 1/[\s^2^(F) + 0.001F^2^]'
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^(F) +
0.001F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3041(1)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C27 H27.5 O2 N2.5 Cl1 P2 F6 Re1'
_cod_database_code               4322737