A hybrid imidazolylidene/imidazolium nickel NHC complex: an isolated intermediate.
Altmann, Philipp J.; Ehrenreich, Michael; Pöthig, Alexander; Acta crystallographica. Section C, Structural chemistry 73 (2017) 880–884; doi:10.1107/S2053229617013250

data_2311934
_publ_section_title
;
 A hybrid imidazolylidene/imidazolium nickel NHC complex: an isolated
 intermediate.
;
_journal_coeditor_code           FP3043
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              880
_journal_page_last               884
_journal_paper_doi               10.1107/S2053229617013250
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ni3 (C24 H24 N12)2 Cl2] (P F6)4, 4C2 H3 N'
_chemical_formula_moiety
'C48 H48 Cl2 N24 Ni3 4+, 4(F6 P -), 4(C2 H3 N)'
_chemical_formula_sum            'C56 H60 Cl2 F24 N28 Ni3 P4'
_chemical_formula_weight         1952.17
_chemical_name_systematic
'Di-\m-chlorido-bis{\m-calix[2]imidazolium[2]imidazolylidene[2]pyrazolate}trinickel(II) tetrakis(hexafluoridophosphate) acetonitrile tetrasolvate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                66.056(3)
_cell_angle_beta                 73.926(3)
_cell_angle_gamma                65.297(3)
_cell_formula_units_Z            1
_cell_length_a                   11.8775(9)
_cell_length_b                   13.3374(9)
_cell_length_c                   13.9741(9)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.9702
_cell_measurement_theta_min      2.3273
_cell_volume                     1822.6(2)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
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PLATON (Spek, 2009), Mercury (Macrae <i>et al.</i>,  2008)
;
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PLATON (Spek, 2009), enCIFer (Allen <i>et al.</i>,  2004)
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_computing_structure_refinement
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SHELXL2014 (Sheldrick, 2015), SHELXLE (H\"ubschle <i>et al.</i>,
2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51283
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         29.13
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_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2014/5, Bruker, 2014
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.774
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0381P)^2^+2.3353P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                7472
_reflns_number_total             9819
_reflns_threshold_expression     I>2\s(I)
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_cod_original_cell_volume        1822.7(2)
_cod_database_code               2311934
_shelx_hkl_checksum              873
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