Synthesis of Enantiopure Oxorhenium(V) and Arylimidorhenium(V) "3 + 2" Schiff Base Complexes. X-ray Diffraction, Cyclic Voltammetry, UV-Vis, and Circular Dichroism Characterizations
Virginie M. Béreau; Saeed I. Khan; Mahdi M. Abu-Omar; Inorganic Chemistry 40 (2001) 6767–6773; doi:10.1021/ic0108033

data_4320740
_publ_section_title
;
 Synthesis of Enantiopure Oxorhenium(V) and Arylimidorhenium(V) "3 + 2"
 Schiff Base Complexes. X-ray Diffraction, Cyclic Voltammetry, UV-Vis, and
 Circular Dichroism Characterizations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6767
_journal_page_last               6773
_journal_paper_doi               10.1021/ic0108033
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H38 N3 O5 Re'
_chemical_formula_weight         826.93
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.817(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.286(3)
_cell_length_b                   18.759(6)
_cell_length_c                   9.957(3)
_cell_measurement_reflns_used    892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.121
_cell_measurement_theta_min      4.995
_cell_volume                     1691.3(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11169
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0.004
_exptl_absorpt_coefficient_mu    3.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.865777
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs(Bruker)
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             828
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.801
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0046P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                5827
_reflns_number_total             6725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0108033_2.cif
_cod_data_source_block           Compound(5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1691.3(10)
_cod_database_code               4320740