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_4347796
_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
'0.78(C20 H21 B N8 O Re), 0.22(C19 H17 B Cl N8 Re)'
_chemical_formula_sum            'C19.78 H20.35 B Cl0.22 N8 O0.78 Re'
_chemical_formula_weight         587.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                9623
_audit_creation_date             2015-09-22
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.558(3)
_cell_length_b                   14.386(2)
_cell_length_c                   9.793(2)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3275
_cell_measurement_theta_min      2.8319
_cell_volume                     2051.0(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            62065
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.345
_diffrn_reflns_theta_min         2.879
_exptl_absorpt_coefficient_mu    5.983
_exptl_absorpt_correction_T_max  0.68579
_exptl_absorpt_correction_T_min  0.41818
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.988
_refine_diff_density_min         -2.848
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+3.6606P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3361
_reflns_number_total             3781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00609_si_002.cif
_cod_data_source_block           7
_cod_database_code               4347796
_shelx_estimated_absorpt_t_min   0.510
_shelx_estimated_absorpt_t_max   0.615
_shelx_res_checksum              11008