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_4345029
_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_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
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9530(6)
_cell_length_b                   15.1091(12)
_cell_length_c                   16.3803(12)
_cell_measurement_reflns_used    5964
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.49
_cell_volume                     1968.3(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction
; 
SAINT V7.23A, 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      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \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  bm69t2as
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24754
_diffrn_reflns_theta_full        27.29
_diffrn_reflns_theta_max         27.29
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    6.345
_exptl_absorpt_correction_T_max  0.5401
_exptl_absorpt_correction_T_min  0.3485
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1144
_exptl_crystal_id                bm69t2as
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -2 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack (1983),  1885 Friedels'
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0239P)^2^+0.0835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4114
_reflns_number_total             4412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b03076_si_003.cif
_cod_data_source_block           N,N-cis_Re(O)(hox)2Cl_(8b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4345027--4345029.cif.
;
_cod_database_code               4345029