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_4345027
_publ_contact_author
; 
Jinyong Liu and Timothy J. Strathmann
Colorado School of Mines
Department of Civil and Environmental Engineering
Golden, Colorado  80401 
USA 
;
_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         'C20 H20 Cl N2 O5 Re'
_chemical_formula_sum            'C20 H20 Cl N2 O5 Re'
_chemical_formula_weight         590.03
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.2324(4)
_cell_length_b                   11.2324(4)
_cell_length_c                   27.4564(12)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.57
_cell_volume                     3000.0(2)
_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 V2014/4, 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-2014-7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  cd94q2sa
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            107510
_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         29.573
_diffrn_reflns_theta_min         2.221
_exptl_absorpt_coefficient_mu    6.244
_exptl_absorpt_correction_T_max  0.78222
_exptl_absorpt_correction_T_min  0.55895
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1716
_exptl_crystal_id                cd94q2sa
_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          0.176
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.627
_refine_diff_density_min         -2.163
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack (1983),  2739 Friedels'
_refine_ls_abs_structure_Flack   -0.012(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+4.8835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5395
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03076_si_003.cif
_cod_data_source_block           N,N-trans_Re(O)(Mehoz)2Cl_(4a)
_cod_depositor_comments
'Adding full bibliography for 4345027--4345029.cif.'
_cod_original_cell_volume        3000.0(3)
_cod_database_code               4345027
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.406
_shelx_estimated_absorpt_t_max   0.745
_shelx_res_checksum              24639
_shelx_hkl_checksum              82218