Redox Activity of Noninnocent 2,2′-Bipyridine in Zinc Complexes: An Experimental and Theoretical Study
Li, Bin; Geoghegan, Blaise L.; Wölper, Christoph; Cutsail, George E.; Schulz, Stephan; ACS Omega  (2021) –; doi:10.1021/acsomega.1c02201

data_4518865
_publ_section_title
;
 Redox Activity of Noninnocent 2,2&#x2032;-Bipyridine in Zinc Complexes:
 An Experimental and Theoretical Study
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.1c02201
_journal_year                    2021
_chemical_formula_sum            'C64 H93 K N6 O6 Zn'
_chemical_formula_weight         1146.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   diffamp
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                92.842(7)
_cell_angle_beta                 101.515(7)
_cell_angle_gamma                100.685(7)
_cell_formula_units_Z            2
_cell_length_a                   12.0286(18)
_cell_length_b                   15.196(2)
_cell_length_c                   17.896(3)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.31
_cell_volume                     3137.0(8)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX3(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/QUEEN'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            128595
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.727
_diffrn_reflns_theta_min         1.369
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.591
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         19357
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+4.4727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13445
_reflns_number_total             19357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02201_si_002.cif
_cod_data_source_block           lb_181m
_cod_database_code               4518865
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              7323
_shelx_hkl_checksum              16868