Synthesis and complexation of superbulky imidazolium-2-dithiocarboxylate ligands
Beltrán, Tomás F.; Zaragoza, Guillermo; Delaude, Lionel; Dalton Trans.  (2017) –; doi:10.1039/C7DT01889D

data_7043419
_publ_section_title
;
 Synthesis and complexation of superbulky imidazolium-2-dithiocarboxylate
 ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01889D
_journal_year                    2017
_chemical_formula_moiety         'C70 H56 N2 S2'
_chemical_formula_sum            'C70 H56 N2 S2'
_chemical_formula_weight         989.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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             2017-03-03T10:30:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-05-08 deposited with the CCDC.
2017-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.491(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4144(15)
_cell_length_b                   16.6967(16)
_cell_length_c                   25.6311(23)
_cell_measurement_reflns_used    1964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.82
_cell_measurement_wavelength     0.71073
_cell_volume                     5558.1(10)
_computing_cell_refinement       'APPEX2v2014.11-0 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2v2014.11-0 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2v2014.11-0 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'DIRDIF2008 (Beurskens et al, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.057459
_diffrn_orient_matrix_UB_12      -0.039845
_diffrn_orient_matrix_UB_13      0.008409
_diffrn_orient_matrix_UB_21      0.037902
_diffrn_orient_matrix_UB_22      0.031661
_diffrn_orient_matrix_UB_23      -0.022017
_diffrn_orient_matrix_UB_31      0.034502
_diffrn_orient_matrix_UB_32      0.031576
_diffrn_orient_matrix_UB_33      0.032687
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64548
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.14
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+4.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0
_reflns_number_gt                8230
_reflns_number_total             11365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01889d2.cif
_cod_data_source_block           NIHO11
_cod_database_code               7043419
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              74933