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_4320739
_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            'C33 H29 Cl2 N2 O5 Re'
_chemical_formula_weight         790.68
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5599(16)
_cell_length_b                   9.9579(16)
_cell_length_c                   31.712(5)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.482
_cell_measurement_theta_min      6.046
_cell_volume                     3018.9(8)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            19818
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0.005
_exptl_absorpt_coefficient_mu    4.247
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs (Bruker)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.247
_refine_diff_density_min         -2.276
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+5.2071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                6932
_reflns_number_total             7155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0108033_1.cif
_cod_data_source_block           Compound(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        3018.9(9)
_cod_database_code               4320739