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_7122008
_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         'C27 H54 Cd N3 S6, C12 H28 N, C3 H6 O'
_chemical_formula_sum            'C42 H88 Cd N4 O S6'
_chemical_formula_weight         969.92
_chemical_name_common            (Pr4N)[Cd((iBu)2dtc)3].(CH3)CO
_chemical_name_systematic
'tetrapropyammonium cadmium tris(diisobutyldithiocarbonate)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.093(4)
_cell_length_b                   22.769(5)
_cell_length_c                   10.847(2)
_cell_measurement_reflns_used    6530
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.033
_cell_volume                     5209.5(18)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            64215
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.909
_diffrn_reflns_theta_min         2.033
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.693
_exptl_crystal_colour            'colourless transparent'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.664
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 5413 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         12375
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0463P)^2^+5.3245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                11911
_reflns_number_total             12375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03737j2.cif
_cod_data_source_block           8B_CH3CO
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '__reflns_threshold_expression' replaced with
'_reflns_threshold_expression'.

Automatic conversion script
Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas 

 Adding full bibliography for 7122005--7122008.cif.
;
_cod_database_code               7122008
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C39) = Uanis(C39A)
Uanis(C37) = Uanis(C38A)
3. Others
 Fixed Sof: H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) C38A(0.5) H38A(0.5)
 H38B(0.5) C38(0.5) H38C(0.5) H38D(0.5) C39A(0.5) H39A(0.5) H39B(0.5) H39C(0.5)
 C39(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C7(H7), C25(H25), C21(H21), C12(H12), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C24(H24A,H24B), C6(H6A,H6B), C20(H20A,H20B), C31(H31A,H31B),
 C28(H28A,H28B), C34(H34A,H34B), C29(H29A,H29B), C35(H35A,H35B), C11(H11A,H11B),
  C15(H15A,H15B), C32(H32A,H32B), C37(H37A,H37B), C37(H37C,H37D), C38A(H38A,
 H38B), C38(H38C,H38D)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C36(H36A,
 H36B,H36C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C),
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C42(H42A,
 H42B,H42C), C40(H40A,H40B,H40C), C39A(H39A,H39B,H39C), C39(H39D,H39E,H39F)
;
_shelx_res_checksum              74622
_olex2_submission_special_instructions 'No special instructions were received'