Probing the Protonation State and the Redox-Active Sites of Pendant Base Iron(II) and Zinc(II) Pyridinediimine Complexes.
Delgado, Mayra; Sommer, Samantha K.; Swanson, Seth P.; Berger, Robert F.; Seda, Takele; Zakharov, Lev N.; Gilbertson, John D.; Inorganic chemistry 54 (2015) 7239–7248; doi:10.1021/acs.inorgchem.5b00633

data_4346152
_publ_section_title
;
 Probing the Protonation State and the Redox-Active Sites of Pendant Base
 Iron(II) and Zinc(II) Pyridinediimine Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7239
_journal_page_last               7248
_journal_paper_doi               10.1021/acs.inorgchem.5b00633
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C31 H49 Br2 N4 O0.5 Zn'
_chemical_formula_weight         710.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.324(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4818(4)
_cell_length_b                   14.9847(5)
_cell_length_c                   23.9343(9)
_cell_measurement_reflns_used    7040
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      3.48
_cell_volume                     3391.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24722
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.631
_diffrn_reflns_theta_min         3.483
_diffrn_source                   'micro-tube Incoatec I\mS'
_exptl_absorpt_coefficient_mu    3.958
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_platon_squeeze_details
; 
The O(CH2CH3)2 solvent molecule (42 electrons) 
disordred around an inverstion center was treated by 
SQUEEZE.
;
_refine_diff_density_max         3.129
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0922P)^2^+5.2585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4749
_reflns_number_total             5940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00633_si_002.cif
_cod_data_source_block           cu_gilbr172_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C31 H49 Br2 N4 O0.50 Zn'
_cod_database_code               4346152
_shelx_estimated_absorpt_t_min   0.627
_shelx_estimated_absorpt_t_max   0.797
_shelxl_version_number           2013-4
_shelx_res_checksum              23279
_shelx_hkl_checksum              39868