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

data_7043416
_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
'C80 H70 Cl N2 O2 Ru S2, F6 P, 2(C3 H6 O), 0.6(H2 O)'
_chemical_formula_sum            'C86 H83.2 Cl F6 N2 O4.6 P Ru S2'
_chemical_formula_weight         1563.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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             2017-04-06T15:47:27-00:00
_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                 94.809(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2889(15)
_cell_length_b                   18.8666(16)
_cell_length_c                   26.085(3)
_cell_measurement_reflns_used    1976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.60
_cell_measurement_wavelength     0.71073
_cell_volume                     7497.7(13)
_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_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1274
_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       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58064
_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         25.668
_diffrn_reflns_theta_min         1.492
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     988
_refine_ls_number_reflns         14215
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+5.4720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0
_reflns_number_gt                8266
_reflns_number_total             14215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01889d2.cif
_cod_data_source_block           NIHO21b
_cod_original_cell_volume        7497.8(12)
_cod_original_formula_sum        'C86 H83.20 Cl F6 N2 O4.60 P Ru S2'
_cod_database_code               7043416
_shelx_estimated_absorpt_t_min   0.94
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              73160