Electronic Insights into Aminoquinoline-Based PNHN Ligands: Protonation State Dictates Geometry While Coordination Environment Dictates N-H Acidity and Bond Strength
Gradiski, Matthew Viktor; Rennie, Benjamin E.; Lough, Alan; Morris, Robert H.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01556K

data_7710479
_publ_section_title
;
 Electronic Insights into Aminoquinoline-Based PNHN Ligands: Protonation
 State Dictates Geometry While Coordination Environment Dictates N-H
 Acidity and Bond Strength
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01556K
_journal_year                    2022
_chemical_formula_moiety         'C46 H42 Fe N4 P2, 2(B F4), 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H46 B2 Cl4 F8 Fe N4 P2'
_chemical_formula_weight         1112.10
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-12-19 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.179(1)
_cell_angle_beta                 86.803(1)
_cell_angle_gamma                85.563(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0025(4)
_cell_length_b                   13.0919(5)
_cell_length_c                   16.8984(5)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.64
_cell_measurement_theta_min      2.53
_cell_volume                     2415.25(15)
_computing_cell_refinement       APEX3
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78530
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.666
_diffrn_reflns_theta_min         1.211
_diffrn_source                   'sealed tube with Bruker Triumph monochromator'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0337P)^2^+1.9619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7913
_reflns_number_total             11228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01556k2.cif
_cod_data_source_block           d1911_a
_cod_database_code               7710479
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              2094
_shelx_hkl_checksum              25484