Trialkylphosphine-Stabilized Copper(I) Dialkylaluminum(III) Ethanedithiolate Complexes: Single-Source Precursors and a Novel Modification of Copper Aluminum Disulfide.
Kischel, Marcus; Dornberg, Gregor; Krautscheid, Harald; Inorganic chemistry 53 (2014) 1614–1623; doi:10.1021/ic402675w

data_4337389
_publ_section_title
;
 Trialkylphosphine-Stabilized Copper(I) Dialkylaluminum(III)
 Ethanedithiolate Complexes: Single-Source Precursors and a Novel
 Modification of Copper Aluminum Disulfide.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1614
_journal_page_last               1623
_journal_paper_doi               10.1021/ic402675w
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C15 H39 Cu5 P3 S6), C12 H36 Cu P4), 1.5(C4 H8 O)'
_chemical_formula_sum            'C33 H87 Cu6 O1.5 P7 S6'
_chemical_formula_weight         1298.42
_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_date             2013-02-21T15:44:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.368(8)
_cell_angle_beta                 91.008(8)
_cell_angle_gamma                112.984(7)
_cell_formula_units_Z            2
_cell_length_a                   12.0748(11)
_cell_length_b                   14.3899(13)
_cell_length_c                   19.191(2)
_cell_measurement_reflns_used    24972
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      1.55
_cell_measurement_wavelength     0.71073
_cell_volume                     3044.1(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA, STOE X-RED'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_publication_material
;
'WinGX publication routines'
Farrugia, L. J. (1999) WinGX, J. Appl. Cryst. 32, 837-838
;
_computing_structure_refinement
;
'SHELXL-97'
Sheldrick, G.M. (2008) Acta Cryst. A64, 112
;
_computing_structure_solution
;
'SIR-92'
Altomare, A., Cascarano, G., 
Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350.
;
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20744
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.472
_exptl_absorpt_correction_T_max  0.8270
_exptl_absorpt_correction_T_min  0.3182
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and  
Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         10937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                7680
_reflns_number_total             10937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402675w_si_002.cif
_cod_data_source_block           '[(Me3P)4Cu][Cu4(SC2H4S)3Cu(Me3P)3]'
_cod_original_formula_sum        'C33 H87 Cu6 O1.50 P7 S6'
_cod_database_code               4337389