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_7710475
_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_absolute_configuration ad
_chemical_formula_moiety         'C23 H32 Cl Co N2 P'
_chemical_formula_sum            'C23 H32 Cl Co N2 P'
_chemical_formula_weight         461.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-12-19 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.836(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9916(9)
_cell_length_b                   9.4534(10)
_cell_length_c                   16.8751(19)
_cell_measurement_reflns_used    3384
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.27
_cell_measurement_theta_min      2.65
_cell_volume                     1102.1(2)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18447
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.207
_diffrn_reflns_theta_max         67.207
_diffrn_reflns_theta_min         2.650
_diffrn_source                   'Bruker ImuS with multi-layer optics'
_exptl_absorpt_coefficient_mu    7.976
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       needle
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.036(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0648
_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^)+(0.1040P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3059
_reflns_number_total             3837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01556k2.cif
_cod_data_source_block           d18150_a
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7710475
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.381
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              12925
_shelx_hkl_checksum              93542