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_4322739
_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            'C14 H16 Cl2 N3 O2 Re'
_chemical_formula_weight         515.41
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.00(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.577(1)
_cell_length_b                   13.269(2)
_cell_length_c                   9.686(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     816.5(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    ORTEP
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_orient_matrix_UB_11      0.13579
_diffrn_orient_matrix_UB_12      0.02297
_diffrn_orient_matrix_UB_13      0.06553
_diffrn_orient_matrix_UB_21      0.06434
_diffrn_orient_matrix_UB_22      0.00375
_diffrn_orient_matrix_UB_23      -0.08277
_diffrn_orient_matrix_UB_31      -0.04687
_diffrn_orient_matrix_UB_32      0.07168
_diffrn_orient_matrix_UB_33      -0.01667
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2683
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0.02
_diffrn_standards_interval_count 150
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_exptl_absorpt_coefficient_mu    7.780
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            blue
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
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_refine_diff_density_min         -1.03
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.2Ueq(C)'
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2230
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0277
_refine_ls_shift/esd_max         0.0030
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.000001|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0211
_reflns_number_observed          2230
_reflns_number_total             2494
_reflns_observed_criterion       I>2.0sigma(I)
_cod_data_source_file            ic971477n_4.cif
_cod_data_source_block           IC971477N-9-a-0/ReOCl2(bpenO)
_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^(Fo) +
0.000001|Fo|^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^(Fo) + 0.000001|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        816.5(2)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C14 H16 Cl2 N3 O2 Re '
_cod_database_code               4322739