#------------------------------------------------------------------------------
#$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2203203.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2203203
loop_
_publ_author_name
'Margraf, G\"unter'
'Lerner, Hans-Wolfram'
'Wagner, Matthias'
'Bolte, Michael'
_publ_section_title
;
The absolute structure of tetrakis(trimethylphosphine)copper(I)
dichlorocopper(I)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              m186
_journal_page_last               m187
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cu (C3 H9 P4)4] [Cu Cl2]'
_chemical_formula_moiety         'C12 H36 Cu1 P4 1+, Cl2 Cu1 1-'
_chemical_formula_sum            'C12 H36 Cl2 Cu2 P4'
_chemical_formula_weight         502.27
_chemical_name_systematic        
;
;
_symmetry_cell_setting           Cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4832(11)
_cell_length_b                   13.4832(11)
_cell_length_c                   13.4832(11)
_cell_measurement_reflns_used    5949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      3.8
_cell_volume                     2451.2(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-AREA
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Stoe IPDS-II two-circle'
_diffrn_measurement_method       \w
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4186
_diffrn_reflns_theta_full        31.32
_diffrn_reflns_theta_max         31.32
_diffrn_reflns_theta_min         3.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.206
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_process_details   '(MULABS; Spek, 1990; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.368
_refine_ls_abs_structure_details 'Flack (1983), 686 Friedels'
_refine_ls_abs_structure_Flack   -0.012(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         2172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0565P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                2035
_reflns_number_total             2172
_reflns_threshold_expression     I>2\s(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'z, x, y'
'-z+1/2, -x, y+1/2'
'z+1/2, -x+1/2, -y'
'-z, x+1/2, -y+1/2'
'y, z, x'
'y+1/2, -z+1/2, -x'
'-y, z+1/2, -x+1/2'
'-y+1/2, -z, x+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cu1 0.543243(16) 0.543243(16) 0.543243(16) 0.03172(9) Uani d S 1 Cu
P1 0.44661(4) 0.44661(4) 0.44661(4) 0.0444(2) Uani d S 1 P
P2 0.56283(4) 0.69364(4) 0.47078(5) 0.04043(13) Uani d . 1 P
C1 0.4214(5) 0.3225(3) 0.4927(5) 0.0959(16) Uani d . 1 C
H1A 0.3789 0.2872 0.4454 0.144 Uiso calc R 1 H
H1B 0.3876 0.3269 0.5569 0.144 Uiso calc R 1 H
H1C 0.4839 0.2864 0.5007 0.144 Uiso calc R 1 H
C2 0.6560(2) 0.7748(2) 0.5257(3) 0.0580(7) Uani d . 1 C
H2A 0.7195 0.7396 0.5295 0.087 Uiso calc R 1 H
H2B 0.6349 0.7940 0.5925 0.087 Uiso calc R 1 H
H2C 0.6636 0.8342 0.4846 0.087 Uiso calc R 1 H
C3 0.4546(2) 0.7750(2) 0.4689(5) 0.0833(14) Uani d . 1 C
H3A 0.3978 0.7392 0.4409 0.125 Uiso calc R 1 H
H3B 0.4688 0.8334 0.4281 0.125 Uiso calc R 1 H
H3C 0.4389 0.7960 0.5367 0.125 Uiso calc R 1 H
C4 0.6003(5) 0.6932(4) 0.3404(3) 0.0843(13) Uani d . 1 C
H4A 0.5550 0.6510 0.3023 0.127 Uiso calc R 1 H
H4B 0.6680 0.6674 0.3347 0.127 Uiso calc R 1 H
H4C 0.5979 0.7610 0.3143 0.127 Uiso calc R 1 H
Cu2 0.86620(2) 0.86620(2) 0.86620(2) 0.04708(13) Uani d S 1 Cu
Cl1 0.95586(7) 0.95586(7) 0.95586(7) 0.0914(6) Uani d S 1 Cl
Cl2 0.77738(7) 0.77738(7) 0.77738(7) 0.1003(7) Uani d S 1 Cl
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.03172(9) 0.03172(9) 0.03172(9) -0.00126(8) -0.00126(8) -0.00126(8)
P1 0.0444(2) 0.0444(2) 0.0444(2) -0.0078(2) -0.0078(2) -0.0078(2)
P2 0.0357(3) 0.0370(2) 0.0487(3) -0.00312(18) -0.0048(2) 0.0080(2)
C1 0.121(4) 0.0518(17) 0.115(4) -0.037(2) -0.030(3) 0.005(2)
C2 0.0480(13) 0.0481(12) 0.078(2) -0.0162(10) -0.0082(13) 0.0053(13)
C3 0.0450(14) 0.0497(13) 0.155(4) 0.0053(11) -0.015(2) 0.024(2)
C4 0.125(4) 0.077(2) 0.0507(16) -0.012(2) 0.006(2) 0.0215(15)
Cu2 0.04708(13) 0.04708(13) 0.04708(13) -0.00266(12) -0.00266(12) -0.00266(12)
Cl1 0.0914(6) 0.0914(6) 0.0914(6) -0.0242(5) -0.0242(5) -0.0242(5)
Cl2 0.1003(7) 0.1003(7) 0.1003(7) -0.0301(6) -0.0301(6) -0.0301(6)
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
P1 Cu1 P2 . 5 109.570(18)
P1 Cu1 P2 . . 109.569(17)
P2 Cu1 P2 5 . 109.372(17)
P1 Cu1 P2 . 9 109.569(17)
P2 Cu1 P2 5 9 109.373(18)
P2 Cu1 P2 . 9 109.373(18)
C1 P1 C1 5 . 101.9(2)
C1 P1 C1 5 9 101.9(2)
C1 P1 C1 . 9 101.9(2)
C1 P1 Cu1 5 . 116.26(18)
C1 P1 Cu1 . . 116.26(18)
C1 P1 Cu1 9 . 116.26(18)
C2 P2 C3 . . 101.31(18)
C2 P2 C4 . . 101.7(2)
C3 P2 C4 . . 102.1(3)
C2 P2 Cu1 . . 116.23(11)
C3 P2 Cu1 . . 116.76(13)
C4 P2 Cu1 . . 116.35(15)
P1 C1 H1A . . 109.5
P1 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
P1 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
P2 C2 H2A . . 109.5
P2 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
P2 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
P2 C3 H3A . . 109.5
P2 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
P2 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
P2 C4 H4A . . 109.5
P2 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
P2 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
Cl2 Cu2 Cl1 . . 180.00(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 P1 . 2.2567(11)
Cu1 P2 5 2.2663(6)
Cu1 P2 . 2.2664(6)
Cu1 P2 9 2.2664(6)
P1 C1 5 1.818(4)
P1 C1 . 1.818(4)
P1 C1 9 1.818(4)
P2 C2 . 1.823(3)
P2 C3 . 1.826(3)
P2 C4 . 1.829(4)
C1 H1A . 0.9800
C1 H1B . 0.9800
C1 H1C . 0.9800
C2 H2A . 0.9800
C2 H2B . 0.9800
C2 H2C . 0.9800
C3 H3A . 0.9800
C3 H3B . 0.9800
C3 H3C . 0.9800
C4 H4A . 0.9800
C4 H4B . 0.9800
C4 H4C . 0.9800
Cu2 Cl2 . 2.0743(17)
Cu2 Cl1 . 2.0938(16)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
P2 Cu1 P1 C1 5 5 -179.6(3)
P2 Cu1 P1 C1 . 5 60.4(3)
P2 Cu1 P1 C1 9 5 -59.6(3)
P2 Cu1 P1 C1 5 . -59.6(3)
P2 Cu1 P1 C1 . . -179.6(3)
P2 Cu1 P1 C1 9 . 60.4(3)
P2 Cu1 P1 C1 5 9 60.4(3)
P2 Cu1 P1 C1 . 9 -59.6(3)
P2 Cu1 P1 C1 9 9 -179.6(3)
P1 Cu1 P2 C2 . . -169.42(13)
P2 Cu1 P2 C2 5 . 70.46(13)
P2 Cu1 P2 C2 9 . -49.30(14)
P1 Cu1 P2 C3 . . 71.0(2)
P2 Cu1 P2 C3 5 . -49.1(2)
P2 Cu1 P2 C3 9 . -168.9(2)
P1 Cu1 P2 C4 . . -49.7(2)
P2 Cu1 P2 C4 5 . -169.8(2)
P2 Cu1 P2 C4 9 . 70.4(2)
_cod_database_code 2203203