Ligand Design for Isomer-Selective Oxorhenium(V) Complex Synthesis.
Liu, Jinyong; Su, Xiaoge; Han, Mengwei; Wu, Dimao; Gray, Danielle L.; Shapley, John R.; Werth, Charles J.; Strathmann, Timothy J.; Inorganic chemistry 56 (2017) 1757–1769; doi:10.1021/acs.inorgchem.6b03076

data_4345028
_publ_section_title
;
 Ligand Design for Isomer-Selective Oxorhenium(V) Complex Synthesis.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1757
_journal_page_last               1769
_journal_paper_doi               10.1021/acs.inorgchem.6b03076
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H28 Cl N2 O5 Re'
_chemical_formula_sum            'C32 H28 Cl N2 O5 Re'
_chemical_formula_weight         742.21
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4735(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9014(7)
_cell_length_b                   6.8299(3)
_cell_length_c                   15.2612(8)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      3.01
_cell_volume                     1448.50(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd95rsa
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_min         1.957
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.2964
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             732
_exptl_crystal_id                cd95rsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-4 -1 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.089
_refine_diff_density_max         3.006
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack (1983),  3292 Friedels'
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7190
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0205P)^2^+2.4635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6954
_reflns_number_total             7190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03076_si_003.cif
_cod_data_source_block           N,N-trans_Re(O)(Bnhoz)2Cl_(5a)
_cod_depositor_comments
'Adding full bibliography for 4345027--4345029.cif.'
_cod_database_code               4345028
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.313
_shelx_estimated_absorpt_t_max   0.699
_exptl_absorpt_special_details
; 
 The following wavelength and cell were deduced by SADABS from the 
 direction cosines etc. They are given here for emergency use only: 
 CELL 0.71084   13.907    6.832   15.265   90.009   91.480   90.006 
;
_shelx_res_checksum              2846
_shelx_hkl_checksum              8704