Configuration Control in the Synthesis of Homo- and Heteroleptic Bis(oxazolinylphenolato/thiazolinylphenolato) Chelate Ligand Complexes of Oxorhenium(V): Isomer Effect on Ancillary Ligand Exchange Dynamics and Implications for Perchlorate Reduction Catalysis.
Liu, Jinyong; Wu, Dimao; Su, Xiaoge; Han, Mengwei; Kimura, Susana Y.; Gray, Danielle L.; Shapley, John R.; Abu-Omar, Mahdi M; Werth, Charles J.; Strathmann, Timothy J.; Inorganic chemistry 55 (2016) 2597–2611; doi:10.1021/acs.inorgchem.5b02940

data_4347253
_publ_section_title
;
 Configuration Control in the Synthesis of Homo- and Heteroleptic
 Bis(oxazolinylphenolato/thiazolinylphenolato) Chelate Ligand Complexes of
 Oxorhenium(V): Isomer Effect on Ancillary Ligand Exchange Dynamics and
 Implications for Perchlorate Reduction Catalysis.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2597
_journal_page_last               2611
_journal_paper_doi               10.1021/acs.inorgchem.5b02940
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C18 H16 Cl N2 O4 Re S '
_chemical_formula_sum            'C18 H16 Cl N2 O4 Re S'
_chemical_formula_weight         578.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 94.944(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2555(8)
_cell_length_b                   8.0421(7)
_cell_length_c                   24.075(2)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.67
_cell_volume                     1785.3(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm45hsa
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         1.698
_exptl_absorpt_coefficient_mu    7.101
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3678
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS 2012/2 (Bruker, 2013)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_id                cm45hsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 -1 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.632
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0109P)^2^+7.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4025
_reflns_number_total             4465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02940_si_002.cif
_cod_data_source_block           N,N-trans_Re(O)(hoz)(htz)Cl_(7a)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347253
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.722
_shelxl_version_number           2013-4
_shelx_res_checksum              80094
_shelx_hkl_checksum              80846