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_4518863
_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 H49 B F20 N4 Zn'
_chemical_formula_weight         1318.24
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 99.269(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5231(13)
_cell_length_b                   35.876(4)
_cell_length_c                   15.4557(18)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      2.19
_cell_volume                     5758.8(12)
_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      120(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            145011
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.370
_diffrn_reflns_theta_min         1.752
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       plate
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.778
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.197
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         22139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0374P)^2^+4.6023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16928
_reflns_number_total             22139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02201_si_002.cif
_cod_data_source_block           lb_171m
_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_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518863
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.902
_shelx_res_checksum              83547
_shelx_hkl_checksum              43248