Imidazolium-benzimidazolates as convenient sources of donor-functionalised normal and abnormal N-heterocyclic carbenes.
Kureja, Kunal; Zinke, Julian; Bruhn, Clemens; Siemeling, Ulrich; Chemical communications (Cambridge, England) 55 (2019) 9705–9708; doi:10.1039/c9cc05283f

data_7125760
_publ_section_title
;
 Imidazolium-benzimidazolates as convenient sources of
 donor-functionalised normal and abnormal N-heterocyclic carbenes.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9705
_journal_page_last               9708
_journal_paper_doi               10.1039/c9cc05283f
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C27 H32 Cl N4 Ni Rh [+ solvent]'
_chemical_formula_sum            'C27 H32 Cl N4 Ni Rh'
_chemical_formula_weight         609.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-07-08 deposited with the CCDC.	2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.3321(4)
_cell_length_b                   34.3321(4)
_cell_length_c                   10.30900(10)
_cell_measurement_reflns_used    44054
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.49
_cell_measurement_theta_min      1.82
_cell_volume                     12151.1(2)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      ' 2089 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            47405
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.480
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.115
_exptl_absorpt_correction_T_max  0.8413
_exptl_absorpt_correction_T_min  0.6236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32. Absorption correction by Gaussian integration, 
analogous to P. Coppens, published in: F. R. Ahmed (Editor), 
"Crystallographic Computing", Munksgaard, Copenhagen (1970), 
255 - 270.
Scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica 
Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             4992
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         11145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0429P)^2^+15.6706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8878
_reflns_number_total             11145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05283f2.cif
_cod_data_source_block           1sq
_cod_original_cell_volume        12151.1(3)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7125760
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.814
_shelx_estimated_absorpt_t_max   0.862
_shelx_res_checksum              37775
_shelx_fab_checksum              94854