Structural and Spectroscopic Characterization of Rhenium Complexes Containing Neutral, Monoanionic, and Dianionic Ligands of 2,2'-Bipyridines and 2,2':6,2″-Terpyridines: An Experimental and Density Functional Theory (DFT)-Computational Study.
Wang, Mei; Weyhermüller, Thomas; Bill, Eckhard; Ye, Shengfa; Wieghardt, Karl; Inorganic chemistry 55 (2016) 5019–5036; doi:10.1021/acs.inorgchem.6b00609

data_4347793
_publ_section_title
;
 Structural and Spectroscopic Characterization of Rhenium Complexes
 Containing Neutral, Monoanionic, and Dianionic Ligands of
 2,2'-Bipyridines and 2,2':6,2&#x2033;-Terpyridines: An Experimental and
 Density Functional Theory (DFT)-Computational Study.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5019
_journal_page_last               5036
_journal_paper_doi               10.1021/acs.inorgchem.6b00609
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C36 H36 N6 Re, 2(C F3 O3 S), 2(C H4 O)'
_chemical_formula_sum            'C40 H44 F6 N6 O8 Re S2'
_chemical_formula_weight         1101.13
_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_block_code                WGT-WM-094-01
_audit_creation_date             2015-10-06
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.874(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.180(2)
_cell_length_b                   19.315(3)
_cell_length_c                   17.588(2)
_cell_measurement_reflns_used    9583
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4806
_cell_measurement_theta_min      2.8013
_cell_volume                     4453.9(11)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (G. M. Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         1\mS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            134879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.585
_diffrn_reflns_theta_min         2.556
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.78428
_exptl_absorpt_correction_T_min  0.62653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       prism
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.302
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         14887
_refine_ls_number_restraints     486
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0681P)^2^+16.1178P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12608
_reflns_number_total             14887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00609_si_002.cif
_cod_data_source_block           4a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347793
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.722
_shelx_res_checksum              21459