Cadmium tris(dithiocarbamate) ionic liquids as single source, solvent-free cadmium sulfide precursors.
Macreadie, Lauren K.; Forsyth, Craig M.; Turner, David R.; Chesman, Anthony S. R.; Chemical communications (Cambridge, England) 54 (2018) 8925–8928; doi:10.1039/c8cc03737j

data_7122006
_publ_section_title
;
 Cadmium tris(dithiocarbamate) ionic liquids as single source,
 solvent-free cadmium sulfide precursors.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8925
_journal_page_last               8928
_journal_paper_doi               10.1039/c8cc03737j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C21 H42 Cd N3 S6, C9 H20 N, C3 H6 O'
_chemical_formula_sum            'C33 H68 Cd N4 O S6'
_chemical_formula_weight         841.67
_chemical_name_common
'methylbutylpyrrolidinium cadmium tris(dipropldithiocarbamte)'
_chemical_name_systematic        (C4C1py)[Cd((nPr)2dtc)3]
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-29 deposited with the CCDC.
2018-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.564(3)
_cell_length_b                   15.533(3)
_cell_length_c                   18.558(4)
_cell_measurement_reflns_used    10273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.948
_cell_measurement_theta_min      1.739
_cell_volume                     4309.4(16)
_computing_cell_refinement       'XDS (kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips et al. 2002)'
_computing_data_reduction        'XDS (kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44273
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.948
_diffrn_reflns_theta_min         1.739
_diffrn_source                   'Australian Synchrotron MX1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.502
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10273
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0307P)^2^+10.5480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9291
_reflns_number_total             10273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03737j2.cif
_cod_data_source_block           12C_CH3CO
_cod_depositor_comments
'Adding full bibliography for 7122005--7122008.cif.'
_cod_original_cell_volume        4309.5(16)
_cod_database_code               7122006
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 S3, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C36)
4. Others
 Sof(O1)=Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(O2)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C20(H20A,H20B), C24(H24A,H24B), C25(H25A,H25B), C5(H5A,H5B),
 C9(H9A,H9B), C23(H23A,H23B), C2(H2A,H2B), C19(H19A,H19B), C13(H13A,H13B),
 C28(H28A,H28B), C16(H16A,H16B), C26(H26A,H26B), C27(H27A,H27B), C10(H10A,H10B),
  C17(H17A,H17B), C6(H6A,H6B), C3(H3A,H3B), C29(H29A,H29B)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C18(H18A,H18B,
 H18C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C14(H14A,H14B,
 H14C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              99559
_olex2_submission_original_sample_id '(C4C1py)[Cd((nPr)2dtc)3] '
_olex2_submission_special_instructions 'No special instructions were received'