Roles of Hydrogen Bonding in Proton Transfer to κ<sup>P</sup>,κ<sup>N</sup>,κ<sup>P</sup>-N(CH<sub>2</sub>CH<sub>2</sub>P <i> <sup>i</sup> </i> Pr<sub>2</sub>)<sub>2</sub>-Ligated Nickel Pincer Complexes.
Wellala, Nadeesha P. N.; Luebking, John D.; Krause, Jeanette A.; Guan, Hairong; ACS omega 3 (2018) 4986–5001; doi:10.1021/acsomega.8b00777

data_4515984
_publ_section_title
;
 Roles of Hydrogen Bonding in Proton Transfer to
 \k<sup>P</sup>,\k<sup>N</sup>,\k<sup>P</sup>-N(CH<sub>2</sub>CH<sub>2</sub>P
 <i> <sup>i</sup> </i> Pr<sub>2</sub>)<sub>2</sub>-Ligated Nickel Pincer
 Complexes.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              4986
_journal_page_last               5001
_journal_paper_doi               10.1021/acsomega.8b00777
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety
'2(C22 H42 N P2 Ni), Ni Cl4, 4(C6 D6), 0.5(H2 O)'
_chemical_formula_sum            'C68 H85 Cl4 D24 N2 Ni3 O0.5 P4'
_chemical_formula_weight         1428.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 119.3520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.1922(9)
_cell_length_b                   15.3802(4)
_cell_length_c                   17.2936(5)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.91
_cell_measurement_theta_min      3.85
_cell_volume                     7463.2(4)
_computing_cell_refinement       'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2017.3.0 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture Photon-II'
_diffrn_measurement_method       '\w-\f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45614
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.897
_diffrn_reflns_theta_min         4.888
_diffrn_source                   'Incoatec Cu-microfocus 3.0'
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2 (L.Krause, et al. J. Appl. Cryst. (2015), 48, 3-10'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       needle
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7653
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0587P)^2^+5.7992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6722
_reflns_number_total             7653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00777_si_002.cif
_cod_data_source_block           '[2H]2NiCl4'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C68 H85 Cl4 D24 N2 Ni3 O0.50 P4'
_cod_database_code               4515984
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.400
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              86568
_shelx_hkl_checksum              33770