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_4347795
_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         'C30 H22 N6 Re, Cl, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C32.5 H27 Cl6 N6 Re'
_chemical_formula_weight         900.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_code                WGT-WM-063-01
_audit_creation_date             2014-03-13
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.754(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5197(9)
_cell_length_b                   21.126(2)
_cell_length_c                   20.0004(14)
_cell_measurement_reflns_used    212236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1
_cell_measurement_theta_min      2.6289
_cell_volume                     6833.7(9)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            194722
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.148
_diffrn_reflns_theta_min         2.631
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.74692
_exptl_absorpt_correction_T_min  0.57938
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       prism
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.945
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         26005
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+21.9544P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20708
_reflns_number_total             26005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00609_si_002.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C32.50 H27 Cl6 N6 Re'
_cod_database_code               4347795
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.737
_shelx_res_checksum              18159