Interaction of an imidazolium-2-amidinate (NHC-CDI) zwitterion with zinc dichloride in dichloromethane: role as ligands and C-Cl activation promoters.
Sánchez-Roa, David; Santiago, Tomás G; Fernández-Millán, Maria; Cuenca, Tomás; Palma, Pilar; Cámpora, Juan; Mosquera, Marta E. G.; Chemical communications (Cambridge, England) 54 (2018) 12586–12589; doi:10.1039/c8cc07661h

data_1550040
_publ_section_title
;
 Interaction of an imidazolium-2-amidinate (NHC-CDI) zwitterion with zinc
 dichloride in dichloromethane: role as ligands and C-Cl activation
 promoters.
;
_journal_issue                   89
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12586
_journal_page_last               12589
_journal_paper_doi               10.1039/c8cc07661h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C138 H148 Br8 Cl4 N12 Zn2'
_chemical_formula_weight         2886.5
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-09-22T18:47:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-09-22 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                78.121(7)
_cell_angle_beta                 77.607(10)
_cell_angle_gamma                60.899(8)
_cell_formula_units_Z            2
_cell_length_a                   17.6822(15)
_cell_length_b                   17.7483(17)
_cell_length_c                   25.194(3)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.03
_cell_measurement_theta_min      2.78
_cell_measurement_wavelength     0.71073
_cell_volume                     6699.7(13)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.1856
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63267
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        24.787
_diffrn_reflns_theta_max         24.787
_diffrn_reflns_theta_min         3.043
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.48
_platon_squeeze_details
;
There are 8 PhBr per molecular compound, four of them 
presented severe disorder and it was not possible to get a 
chemical sensible model for it, so Squeeze procedure was used to remove 
its contribution to the structure factors.
;
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         21472
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1053P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0
_reflns_number_gt                9508
_reflns_number_total             21472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07661h2.cif
_cod_data_source_block           1_8PhBr
_cod_depositor_comments
'Adding full bibliography for 1550040--1550043.cif.'
_cod_database_code               1550040