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_4515983
_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         'C22 H42 N P2 Ni, C24 H20 B, 1.5(C4 H8 O)'
_chemical_formula_sum            'C52 H74 B N Ni O1.5 P2'
_chemical_formula_weight         868.58
_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                 102.298(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.872(3)
_cell_length_b                   12.8733(14)
_cell_length_c                   32.405(3)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.32
_cell_volume                     9729.9(19)
_computing_cell_refinement       'Bruker SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 v2016.5.0 (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT v8.37A (Bruker, 2015)'
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_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Bruker TRIUMPH curved-graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            77427
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         1.746
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016.2 (Sheldrick, 2016)'
_exptl_crystal_colour            'colorless-blue dichroic'
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       tablet
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9929
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+17.1405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7105
_reflns_number_total             9929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00777_si_002.cif
_cod_data_source_block           '[2H]BPh4'
_cod_original_cell_volume        9730(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C52 H74 B N Ni O1.50 P2'
_cod_database_code               4515983
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              23510
_shelx_hkl_checksum              57153