Crystal structure and DFT analyses of a pentacoordinated PCP pincer nickel(II) complex
Subramaniyan, Vasudevan; Kumar, Ashok; Govindaraj, Anbarasu; Mani, Ganesan; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619006211

data_2021643
_publ_section_title
;
 Crystal structure and DFT analyses of a pentacoordinated PCP pincer
 nickel(II) complex
;
_journal_coeditor_code           KY3175
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619006211
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Ni (C9 H9 N1) (C30 H30 Cl N2 P2)] P F6, 0.7H2 O'
_chemical_formula_moiety         'C39 H39 Cl N3 Ni P2 +, F6 P -, 0.7(H2 O)'
_chemical_formula_sum            'C39 H40.41 Cl F6 N3 Ni O0.7 P3'
_chemical_formula_weight         863.42
_chemical_name_systematic
;{1,3-Bis[(diphenylphosphanyl)methyl]hexahydropyrimidin-2-yl-\k<i>N</i>^2^}(2,6-dimethylphenyl isocyanide-\k<i>C</i>)nickel(II)
hexafluoridophosphate 0.70-hydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                99.6870(10)
_cell_angle_beta                 91.5040(10)
_cell_angle_gamma                93.4720(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7632(5)
_cell_length_b                   10.8846(5)
_cell_length_c                   18.5771(9)
_cell_measurement_reflns_used    24485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.997
_cell_measurement_theta_min      1.902
_cell_volume                     1941.11(16)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24485
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       prism
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         7473
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0324P)^2^+1.1895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                6603
_reflns_number_total             7473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3175sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C39 H40.41 Cl F6 N3 Ni O0.70 P3'
_cod_database_code               2021643
_shelx_estimated_absorpt_t_min   0.679
_shelx_estimated_absorpt_t_max   0.746
_shelx_hkl_checksum              19015
_shelx_res_checksum              71605
_cod_database_fobs_code 2021643