Hydrogen-bonded nickel(I) complexes.
Wilson, Jessica R.; Zeller, Matthias; Szymczak, Nathaniel K.; Chemical communications (Cambridge, England) 57 (2021) 753–756; doi:10.1039/d0cc07216h

data_7127682
_publ_section_title
;
 Hydrogen-bonded nickel(I) complexes.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              753
_journal_page_last               756
_journal_paper_doi               10.1039/d0cc07216h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C18 H18 Cl2 N4 Ni, C2 H3 N'
_chemical_formula_sum            'C20 H21 Cl2 N5 Ni'
_chemical_formula_weight         461.03
_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-2018/3
_audit_update_record
;
2020-10-29 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9491(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.7389(5)
_cell_length_b                   15.7231(8)
_cell_length_c                   30.6187(14)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.1384
_cell_measurement_theta_min      2.4347
_cell_volume                     4206.5(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Apex3 v2018.7-2 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1030 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            43700
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.184
_diffrn_reflns_theta_min         2.379
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, Et2O'
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 11971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         30115
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0228P)^2^+0.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                27587
_reflns_number_total             30115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07216h2.cif
_cod_data_source_block           JRW3203_0m
_cod_depositor_comments
'Adding full bibliography for 7127678--7127684.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7127682
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              81632