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

data_7043414
_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 O2 S2'
_chemical_formula_sum            'C70 H56 N2 O2 S2'
_chemical_formula_weight         1021.28
_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             2017-03-03T12:27:35-00:00
_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                 93.995(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1812(11)
_cell_length_b                   10.1211(8)
_cell_length_c                   35.9635(27)
_cell_measurement_reflns_used    1971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.42
_cell_measurement_wavelength     0.71073
_cell_volume                     5512.4(7)
_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      -0.014101
_diffrn_orient_matrix_UB_12      -0.096428
_diffrn_orient_matrix_UB_13      0.0008
_diffrn_orient_matrix_UB_21      -0.03464
_diffrn_orient_matrix_UB_22      0.015045
_diffrn_orient_matrix_UB_23      0.022272
_diffrn_orient_matrix_UB_31      -0.054418
_diffrn_orient_matrix_UB_32      0.01541
_diffrn_orient_matrix_UB_33      -0.016741
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            47897
_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         26.373
_diffrn_reflns_theta_min         1.345
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.862
_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    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     687
_refine_ls_number_reflns         11269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0828P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0
_reflns_number_gt                6636
_reflns_number_total             11269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01889d2.cif
_cod_data_source_block           NIHO12
_cod_database_code               7043414
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              39046