Novel imidazolium and imidazolinium salts containing the 9-nickelafluorenyl anion - synthesis, structures and reactivity.
Buchalski, Piotr; Pacholski, Roman; Chodkiewicz, Krzysztof; Buchowicz, Włodzimierz; Suwińska, Kinga; Shkurenko, Aleksander; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7169–7176; doi:10.1039/c4dt03786c

data_7034327
_publ_section_title
;
 Novel imidazolium and imidazolinium salts containing the
 9-nickelafluorenyl anion - synthesis, structures and reactivity.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7169
_journal_page_last               7176
_journal_paper_doi               10.1039/c4dt03786c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H40 N2 Ni, 2(C4 H8 O)'
_chemical_formula_sum            'C46 H56 N2 Ni O2'
_chemical_formula_weight         727.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0713(2)
_cell_length_b                   24.610(2)
_cell_length_c                   16.8975(5)
_cell_measurement_reflns_used    3057
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.448
_cell_measurement_theta_min      2.919
_cell_volume                     3772.3(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'SuperNova, Dual, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14432
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.786
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

CrysAlisPro, Agilent Technologies,
 
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
 
(compiled Jul 11 2012,15:38:31)
 
Empirical absorption correction using spherical harmonics,
 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0791P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.851
_reflns_Friedel_fraction_max     0.665
_reflns_number_gt                6023
_reflns_number_total             8281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03786c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7034327--7034332.cif.'
_cod_original_cell_volume        3772.2(3)
_cod_database_code               7034327
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
_shelx_res_checksum              12167