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_4518866
_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            'C63 H97 K N6 O7.5 Zn'
_chemical_formula_weight         1162.93
_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   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                93.949(5)
_cell_angle_beta                 100.383(5)
_cell_angle_gamma                104.210(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5804(14)
_cell_length_b                   17.603(2)
_cell_length_c                   18.015(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.23
_cell_volume                     3176.7(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0818
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.617
_diffrn_reflns_theta_min         2.120
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 TWINABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         16255
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0736P)^2^+3.8951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13112
_reflns_number_total             16255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02201_si_002.cif
_cod_data_source_block           lb_181b_tw5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C63 H97 K N6 O7.50 Zn'
_cod_database_code               4518866
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              24859
_shelx_hkl_checksum              84235