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_4515978
_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         'C16 H37 N Br P2 Ni, Br'
_chemical_formula_sum            'C16 H37 Br2 N Ni P2'
_chemical_formula_weight         523.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 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                 90.049(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6545(8)
_cell_length_b                   10.9830(9)
_cell_length_c                   23.2849(19)
_cell_measurement_reflns_used    7161
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.24
_cell_volume                     2213.3(3)
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1.0'
_computing_data_reduction        'Bruker SAINT v8.37A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material
'Bruker SHELXTL v6.14 & SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement
'Bruker SHELXTL v6.14 & SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'combination of \w and \f-scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.1178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.070
_diffrn_reflns_theta_min         1.907
_exptl_absorpt_coefficient_mu    5.737
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       rod
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be
 determined.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9105
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0123P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6740
_reflns_number_total             9105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00777_si_002.cif
_cod_data_source_block           '[1H]Br'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4515978
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              24607
_shelx_hkl_checksum              48686