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_4515977
_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 H34 Br N Ni P2'
_chemical_formula_sum            'C16 H34 Br N Ni P2'
_chemical_formula_weight         441.00
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.6912(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7169(9)
_cell_length_b                   14.4134(12)
_cell_length_c                   13.8384(11)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      40.19
_cell_measurement_theta_min      2.81
_cell_volume                     2100.5(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)'
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'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 0.992
_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     1.0333
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24534
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        38.315
_diffrn_reflns_theta_max         40.202
_diffrn_reflns_theta_min         2.177
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.253(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                7623
_reflns_number_total             8336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b00777_si_002.cif
_cod_data_source_block           1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4515977
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              90476
_shelx_hkl_checksum              47149