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_4337390
_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_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H70 Al2 Cu2 P2 S4'
_chemical_formula_sum            'C30 H70 Al2 Cu2 P2 S4'
_chemical_formula_weight         802.08
_chemical_name_systematic
;
  bis(\m~3~-1,2-dithiolatoethane-S,S,S',S')-tetraethanido
-bis(triisopropylphosphine)-dicopper(+1)-dialuminium(+3)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-29T18:31:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.840(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0435(8)
_cell_length_b                   15.2761(11)
_cell_length_c                   13.2147(11)
_cell_measurement_reflns_used    11637
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.35
_cell_measurement_wavelength     0.71073
_cell_volume                     2122.1(3)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11029
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.8493
_exptl_absorpt_correction_T_min  0.7010
_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    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), 4276 Friedel pairs'
_refine_ls_abs_structure_Flack   0.462(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8075
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                6717
_reflns_number_total             8075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402675w_si_004.cif
_cod_data_source_block           '[iPr3PCuSC2H4SAlEt2]2'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4337390