New organometallic single-source precursors for CuGaS(2)- polytypism in gallite nanocrystals obtained by thermolysis.
Kluge, Oliver; Friedrich, Dirk; Wagner, Gerald; Krautscheid, Harald; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8635–8642; doi:10.1039/c2dt30904a

data_7019636
_publ_section_title
;
 New organometallic single-source precursors for CuGaS(2)- polytypism in
 gallite nanocrystals obtained by thermolysis.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8635
_journal_page_last               8642
_journal_paper_doi               10.1039/c2dt30904a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H66 Cu2 Ga2 P2 S6, 2(C4 H8 O)'
_chemical_formula_sum            'C44 H82 Cu2 Ga2 O2 P2 S6'
_chemical_formula_weight         1163.92
_chemical_name_systematic
;
bis(\m~2~-ethane-1,2-disulfido)-bis(triisopropylphosphine)-bis(phenylsulfido)-dimethyl-di-copper-di-gallium tetrahydrofuran solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.290(7)
_cell_angle_beta                 72.432(8)
_cell_angle_gamma                65.161(7)
_cell_formula_units_Z            1
_cell_length_a                   10.5998(10)
_cell_length_b                   11.5070(11)
_cell_length_c                   13.6932(15)
_cell_measurement_reflns_used    15556
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.64
_cell_volume                     1378.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 92'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      ' 273 frames, detector distance = 110 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11622
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.64
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  0.8966
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                3829
_reflns_number_total             5374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30904a.txt
_cod_data_source_block           5
_cod_original_cell_volume        1378.6(2)
_cod_database_code               7019636