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_4322736
_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            'C8 H10 Cl2 N2 O2 Re'
_chemical_formula_weight         423.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 100.627(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.632(1)
_cell_length_b                   9.288(1)
_cell_length_c                   14.802(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      12.6
_cell_volume                     1166.4(2)
_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      -0.00517
_diffrn_orient_matrix_UB_12      0.02702
_diffrn_orient_matrix_UB_13      0.06477
_diffrn_orient_matrix_UB_21      0.10656
_diffrn_orient_matrix_UB_22      0.04541
_diffrn_orient_matrix_UB_23      0.00684
_diffrn_orient_matrix_UB_31      -0.05010
_diffrn_orient_matrix_UB_32      0.09380
_diffrn_orient_matrix_UB_33      -0.02197
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3716
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        -2.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
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_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.378
_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
_exptl_crystal_F_000             788.00
_exptl_crystal_size_max          0.40
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_refine_diff_density_max         1.20
_refine_diff_density_min         -1.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.772
_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.2Ueq(C)'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
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_refine_ls_number_reflns         2835
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00000225|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0250
_reflns_number_observed          2835
_reflns_number_total             3596
_reflns_observed_criterion       I>2.0sigma(I)
_cod_data_source_file            ic971477n_1.cif
_cod_data_source_block           IC971477N-9-a-0/ReOCl2(mpenO)
_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) +
0.00000225|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) + 0.00000225|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1166.5(2)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C8 H10 Cl2 N2 O2 Re '
_cod_database_code               4322736