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_4347254
_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 H18 N2 O6 Re, C F3 O3 S'
_chemical_formula_sum            'C19 H18 F3 N2 O9 Re S'
_chemical_formula_weight         693.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                108.1620(10)
_cell_angle_beta                 93.3860(10)
_cell_angle_gamma                99.3290(10)
_cell_formula_units_Z            4
_cell_length_a                   11.8818(3)
_cell_length_b                   13.6186(4)
_cell_length_c                   14.7507(4)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.50
_cell_volume                     2222.61(11)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm57vas
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.507
_diffrn_reflns_theta_min         1.463
_exptl_absorpt_coefficient_mu    5.642
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.1558
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_id                bm57vas
_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 -4 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         8247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^+2.0509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7611
_reflns_number_total             8247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02940_si_002.cif
_cod_data_source_block           C2_[Re(O)(hoz)2(OH2)][OTf]
_cod_database_code               4347254
_shelx_estimated_absorpt_t_min   0.179
_shelx_estimated_absorpt_t_max   0.849
_shelxl_version_number           2014/6
_shelx_res_checksum              34514
_shelx_hkl_checksum              17248