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_4347791
_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         'C51 H41 Cl N3 P2 Re, Cl, 4(C H4 O)'
_chemical_formula_sum            'C55 H57 Cl2 N3 O4 P2 Re'
_chemical_formula_weight         1143.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_block_code                WGT-WM-071-01
_audit_creation_date             2014-04-29
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.640(2)
_cell_length_b                   22.476(2)
_cell_length_c                   25.573(3)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9258
_cell_measurement_theta_min      2.8043
_cell_volume                     10139.1(19)
_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 0.998
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            292290
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.036
_diffrn_reflns_theta_min         2.605
_diffrn_source                   1\mS
_exptl_absorpt_coefficient_mu    2.614
_exptl_absorpt_correction_T_max  0.90964
_exptl_absorpt_correction_T_min  0.80415
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         16178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+21.7040P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12368
_reflns_number_total             16178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00609_si_002.cif
_cod_data_source_block           2
_cod_database_code               4347791
_shelxl_version_number           2013-2
_shelx_res_checksum              93204