#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:19:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179476 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/73/4337392.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4337392
loop_
_publ_author_name
'Kischel, Marcus'
'Dornberg, Gregor'
'Krautscheid, Harald'
_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 H41 Al1 Cu1 P3 S2'
_chemical_formula_sum            'C15 H41 Al Cu P3 S2'
_chemical_formula_weight         469.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-23T15:07:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.901(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8223(12)
_cell_length_b                   16.9838(13)
_cell_length_c                   14.2081(16)
_cell_measurement_reflns_used    17062
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     2610.1(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      213(2)
_diffrn_detector                 'image plate'
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '1-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       'φ 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  0.0941
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24532
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.6247
_exptl_absorpt_correction_T_min  0.3028
_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    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0316
_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/[σ²(Fo²)+(0.0318P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                3585
_reflns_number_total             4852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402675w_si_011.cif
_cod_data_source_block           '[(Me3P)3CuSC2H4SAlEt2]'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4337392
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.2349(3) 0.98166(19) 0.6484(2) 0.0587(8) Uani 1 1 d .
H1A H 0.2032 1.0328 0.6687 0.07 Uiso 1 1 calc R
H1B H 0.3144 0.9911 0.6193 0.07 Uiso 1 1 calc R
C2 C 0.1456(3) 0.9480(2) 0.5742(2) 0.0740(10) Uani 1 1 d .
H2A H 0.1799 0.9001 0.5486 0.111 Uiso 1 1 calc R
H2B H 0.1324 0.9861 0.524 0.111 Uiso 1 1 calc R
H2C H 0.0674 0.9362 0.6026 0.111 Uiso 1 1 calc R
C3 C 0.3467(3) 0.9704(2) 0.8698(2) 0.0713(9) Uani 1 1 d .
H3A H 0.2822 0.9887 0.9114 0.086 Uiso 1 1 calc R
H3B H 0.3968 0.9318 0.9052 0.086 Uiso 1 1 calc R
C4 C 0.4280(4) 1.0394(2) 0.8488(3) 0.0847(11) Uani 1 1 d .
H4A H 0.4928 1.0228 0.8077 0.127 Uiso 1 1 calc R
H4B H 0.4647 1.0596 0.9071 0.127 Uiso 1 1 calc R
H4C H 0.3789 1.0803 0.8181 0.127 Uiso 1 1 calc R
C5 C 0.2591(2) 0.72993(17) 0.76459(19) 0.0488(6) Uani 1 1 d .
H5A H 0.2683 0.6778 0.7362 0.059 Uiso 1 1 calc R
H5B H 0.2867 0.7265 0.8309 0.059 Uiso 1 1 calc R
C6 C 0.1241(2) 0.75451(18) 0.75826(18) 0.0496(7) Uani 1 1 d .
H6A H 0.074 0.714 0.7879 0.06 Uiso 1 1 calc R
H6B H 0.0973 0.7579 0.6918 0.06 Uiso 1 1 calc R
C7 C 0.6295(3) 0.95959(19) 0.6292(2) 0.0659(9) Uani 1 1 d .
H7A H 0.6723 0.9754 0.6873 0.099 Uiso 1 1 calc R
H7B H 0.5422 0.9716 0.633 0.099 Uiso 1 1 calc R
H7C H 0.6635 0.988 0.5768 0.099 Uiso 1 1 calc R
C8 C 0.5886(4) 0.8430(2) 0.49190(19) 0.0879(14) Uani 1 1 d .
H8A H 0.6282 0.8806 0.4514 0.132 Uiso 1 1 calc R
H8B H 0.5001 0.8522 0.4901 0.132 Uiso 1 1 calc R
H8C H 0.6052 0.79 0.4702 0.132 Uiso 1 1 calc R
C9 C 0.8151(3) 0.8479(3) 0.5990(3) 0.0878(12) Uani 1 1 d .
H9A H 0.8378 0.7938 0.5862 0.132 Uiso 1 1 calc R
H9B H 0.857 0.8654 0.6567 0.132 Uiso 1 1 calc R
H9C H 0.8393 0.8812 0.5472 0.132 Uiso 1 1 calc R
C10 C 0.7018(4) 0.8855(2) 0.8977(2) 0.0718(9) Uani 1 1 d .
H10A H 0.7289 0.8857 0.9635 0.108 Uiso 1 1 calc R
H10B H 0.6348 0.9229 0.8881 0.108 Uiso 1 1 calc R
H10C H 0.7702 0.9001 0.859 0.108 Uiso 1 1 calc R
C11 C 0.5423(3) 0.7639(2) 0.95822(19) 0.0712(10) Uani 1 1 d .
H11A H 0.5221 0.7083 0.9559 0.107 Uiso 1 1 calc R
H11B H 0.4673 0.7947 0.9495 0.107 Uiso 1 1 calc R
H11C H 0.5813 0.7764 1.0189 0.107 Uiso 1 1 calc R
C12 C 0.7841(3) 0.7286(2) 0.8986(2) 0.0672(9) Uani 1 1 d .
H12A H 0.8519 0.7427 0.8589 0.101 Uiso 1 1 calc R
H12B H 0.7652 0.6731 0.8907 0.101 Uiso 1 1 calc R
H12C H 0.8074 0.7389 0.9639 0.101 Uiso 1 1 calc R
C13 C 0.5675(4) 0.5688(2) 0.7594(2) 0.0768(10) Uani 1 1 d .
H13A H 0.5693 0.5171 0.7305 0.115 Uiso 1 1 calc R
H13B H 0.489 0.5762 0.7892 0.115 Uiso 1 1 calc R
H13C H 0.6343 0.5731 0.8063 0.115 Uiso 1 1 calc R
C14 C 0.4759(4) 0.6106(2) 0.5782(2) 0.0813(11) Uani 1 1 d .
H14A H 0.4869 0.6409 0.5213 0.122 Uiso 1 1 calc R
H14B H 0.3924 0.6179 0.5994 0.122 Uiso 1 1 calc R
H14C H 0.4897 0.5553 0.5654 0.122 Uiso 1 1 calc R
C15 C 0.7317(4) 0.6158(2) 0.6202(3) 0.0934(13) Uani 1 1 d .
H15A H 0.7311 0.5598 0.6068 0.14 Uiso 1 1 calc R
H15B H 0.7986 0.6278 0.665 0.14 Uiso 1 1 calc R
H15C H 0.7434 0.6449 0.5624 0.14 Uiso 1 1 calc R
Al1 Al 0.26379(7) 0.91466(5) 0.76130(5) 0.04523(19) Uani 1 1 d .
P1 P 0.64924(6) 0.85445(4) 0.61168(4) 0.03897(16) Uani 1 1 d .
P2 P 0.64790(6) 0.78721(4) 0.86502(4) 0.04211(17) Uani 1 1 d .
P3 P 0.58575(7) 0.64385(4) 0.66937(5) 0.04447(17) Uani 1 1 d .
S1 S 0.35482(6) 0.80111(4) 0.70355(4) 0.04158(16) Uani 1 1 d .
S2 S 0.09628(7) 0.84866(5) 0.81474(5) 0.0568(2) Uani 1 1 d .
Cu1 Cu 0.56824(3) 0.770910(18) 0.716825(18) 0.03549(9) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 C1 Al1 115.2(2)
C4 C3 Al1 117.9(2)
C6 C5 S1 110.4(2)
C5 C6 S2 112.9(2)
C1 Al1 C3 114.02(15)
C1 Al1 S2 116.44(10)
C3 Al1 S2 108.52(11)
C1 Al1 S1 104.32(10)
C3 Al1 S1 118.74(12)
S2 Al1 S1 93.47(4)
C9 P1 C8 103.2(2)
C9 P1 C7 101.24(18)
C8 P1 C7 101.17(18)
C9 P1 Cu1 115.78(13)
C8 P1 Cu1 114.64(12)
C7 P1 Cu1 118.47(9)
C11 P2 C10 102.51(18)
C11 P2 C12 102.24(16)
C10 P2 C12 100.58(17)
C11 P2 Cu1 114.88(12)
C10 P2 Cu1 117.22(11)
C12 P2 Cu1 117.02(11)
C15 P3 C14 101.6(2)
C15 P3 C13 101.7(2)
C14 P3 C13 101.48(19)
C15 P3 Cu1 116.52(14)
C14 P3 Cu1 116.57(14)
C13 P3 Cu1 116.40(13)
C5 S1 Al1 97.32(9)
C5 S1 Cu1 112.67(10)
Al1 S1 Cu1 125.08(4)
C6 S2 Al1 98.05(9)
P1 Cu1 P2 113.20(3)
P1 Cu1 P3 111.26(3)
P2 Cu1 P3 111.05(3)
P1 Cu1 S1 102.14(3)
P2 Cu1 S1 112.81(3)
P3 Cu1 S1 105.84(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.518(5)
C1 Al1 1.983(3)
C3 C4 1.500(5)
C3 Al1 1.996(3)
C5 C6 1.519(4)
C5 S1 1.829(3)
C6 S2 1.819(3)
C7 P1 1.817(3)
C8 P1 1.814(3)
C9 P1 1.814(3)
C10 P2 1.823(4)
C11 P2 1.821(3)
C12 P2 1.828(3)
C13 P3 1.821(3)
C14 P3 1.819(4)
C15 P3 1.812(3)
Al1 S2 2.2827(11)
Al1 S1 2.3273(10)
P1 Cu1 2.2584(7)
P2 Cu1 2.2656(7)
P3 Cu1 2.2707(8)
S1 Cu1 2.3674(7)
