#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:19:23 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179055 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/17/4301742.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_4301742
loop_
_publ_author_name
'Scott D. Bunge'
'Jennifer L. Steele'
_publ_contact_author_address
;Kent State University
Chemistry Department
PO Box 5190
Kent, OH 44242, USA
;
_publ_contact_author_email       sbunge@kent.edu
_publ_contact_author_fax         '330 672 3816'
_publ_contact_author_name        'Scott D. Bunge'
_publ_contact_author_phone       '330 672 9445'
_publ_section_title
;
Synthesis and Characterization of Group 11 1,1,3,3-Tetraalkylguanidinate
(TAG) Clusters: [M2(μ-TAG){μ-N(SiMe3)2}]2 (M = Cu, Ag, and Au)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2701
_journal_page_last               2706
_journal_paper_doi               10.1021/ic802291u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C30 H72 Cu4 N8 Si4'
_chemical_formula_weight         911.48
_chemical_name_common            '[Cu2(μ-DEPYRG)2{μ-N(TMS)2}2]2 (4)'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                101.132(7)
_cell_angle_beta                 111.845(4)
_cell_angle_gamma                104.196(5)
_cell_formula_units_Z            1
_cell_length_a                   9.5504(17)
_cell_length_b                   10.6284(17)
_cell_length_c                   12.746(3)
_cell_measurement_reflns_used    7131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.86
_cell_measurement_theta_min      2.29
_cell_volume                     1104.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8461
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.038
_exptl_absorpt_correction_T_max  0.4837
_exptl_absorpt_correction_T_min  0.4378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.708
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0222
_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/[σ²(Fo²)+(0.1000P)²+0.9297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3581
_reflns_number_total             3842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802291u_si_002_4.cif
_cod_data_source_block           js001_tri
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4301742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.07235(3) 0.01796(2) 0.34429(2) 0.02020(11) Uani 1 1 d . . .
Cu2 Cu 0.15305(3) 0.18571(2) 0.56559(2) 0.02013(11) Uani 1 1 d . . .
N1 N 0.2348(2) 0.15940(18) 0.71792(15) 0.0193(3) Uani 1 1 d . . .
N2 N 0.0764(2) 0.19452(18) 0.41192(16) 0.0229(4) Uani 1 1 d . . .
N3 N 0.0720(2) 0.26533(19) 0.24315(16) 0.0268(4) Uani 1 1 d . . .
N4 N 0.1823(3) 0.4253(2) 0.42870(18) 0.0334(5) Uani 1 1 d . . .
Si1 Si 0.41655(7) 0.13250(6) 0.74326(5) 0.02432(15) Uani 1 1 d . . .
Si2 Si 0.20475(7) 0.27120(6) 0.81994(5) 0.02352(15) Uani 1 1 d . . .
C1 C 0.3994(3) 0.0227(3) 0.6026(2) 0.0384(6) Uani 1 1 d . . .
H1A H 0.3111 -0.0645 0.5739 0.058 Uiso 1 1 calc R . .
H1B H 0.5004 0.0057 0.6179 0.058 Uiso 1 1 calc R . .
H1C H 0.3777 0.0693 0.5422 0.058 Uiso 1 1 calc R . .
C2 C 0.4710(4) 0.0431(4) 0.8568(3) 0.0613(10) Uani 1 1 d . . .
H2A H 0.4959 0.1035 0.9348 0.092 Uiso 1 1 calc R . .
H2B H 0.5654 0.0194 0.8607 0.092 Uiso 1 1 calc R . .
H2C H 0.3804 -0.0404 0.8344 0.092 Uiso 1 1 calc R . .
C3 C 0.5847(3) 0.2974(3) 0.7926(3) 0.0473(7) Uani 1 1 d . . .
H3A H 0.5521 0.3499 0.7384 0.071 Uiso 1 1 calc R . .
H3B H 0.6797 0.2785 0.7917 0.071 Uiso 1 1 calc R . .
H3C H 0.6105 0.3502 0.8735 0.071 Uiso 1 1 calc R . .
C4 C -0.0137(3) 0.2487(3) 0.7596(2) 0.0364(6) Uani 1 1 d . . .
H4A H -0.0495 0.2639 0.6819 0.055 Uiso 1 1 calc R . .
H4B H -0.0304 0.3147 0.8148 0.055 Uiso 1 1 calc R . .
H4C H -0.0758 0.1556 0.7504 0.055 Uiso 1 1 calc R . .
C5 C 0.3177(3) 0.4559(2) 0.8492(2) 0.0341(5) Uani 1 1 d . . .
H5A H 0.4312 0.4690 0.8705 0.051 Uiso 1 1 calc R . .
H5B H 0.3092 0.5133 0.9150 0.051 Uiso 1 1 calc R . .
H5C H 0.2717 0.4815 0.7774 0.051 Uiso 1 1 calc R . .
C6 C 0.2729(3) 0.2417(3) 0.9688(2) 0.0345(6) Uani 1 1 d . . .
H6A H 0.2168 0.1465 0.9586 0.052 Uiso 1 1 calc R . .
H6B H 0.2482 0.3028 1.0220 0.052 Uiso 1 1 calc R . .
H6C H 0.3892 0.2606 1.0035 0.052 Uiso 1 1 calc R . .
C7 C 0.1077(3) 0.2881(2) 0.3658(2) 0.0264(5) Uani 1 1 d . . .
C8 C -0.0556(3) 0.3144(3) 0.1780(2) 0.0349(5) Uani 1 1 d . . .
H8A H -0.0584 0.3908 0.2347 0.042 Uiso 1 1 calc R . .
H8B H -0.1610 0.2396 0.1428 0.042 Uiso 1 1 calc R . .
C9 C -0.0302(4) 0.3627(3) 0.0799(2) 0.0475(7) Uani 1 1 d . . .
H9A H 0.0782 0.4305 0.1130 0.071 Uiso 1 1 calc R . .
H9B H -0.1101 0.4043 0.0455 0.071 Uiso 1 1 calc R . .
H9C H -0.0424 0.2846 0.0178 0.071 Uiso 1 1 calc R . .
C10 C 0.0571(3) 0.1311(3) 0.1767(2) 0.0334(5) Uani 1 1 d . . .
H10A H 0.0168 0.1229 0.0911 0.040 Uiso 1 1 calc R . .
H10B H -0.0229 0.0599 0.1854 0.040 Uiso 1 1 calc R . .
C11 C 0.2161(4) 0.1066(3) 0.2190(3) 0.0437(6) Uani 1 1 d . . .
H11A H 0.2965 0.1784 0.2128 0.066 Uiso 1 1 calc R . .
H11B H 0.2018 0.0172 0.1695 0.066 Uiso 1 1 calc R . .
H11C H 0.2526 0.1083 0.3022 0.066 Uiso 1 1 calc R . .
C12 C 0.2215(3) 0.4785(2) 0.5533(2) 0.0364(6) Uani 1 1 d . . .
H12A H 0.2996 0.4425 0.6026 0.044 Uiso 1 1 calc R . .
H12B H 0.1238 0.4546 0.5665 0.044 Uiso 1 1 calc R . .
C13 C 0.2949(4) 0.6322(3) 0.5824(3) 0.0460(7) Uani 1 1 d . . .
H13A H 0.3701 0.6765 0.6680 0.055 Uiso 1 1 calc R . .
H13B H 0.2107 0.6742 0.5608 0.055 Uiso 1 1 calc R . .
C14 C 0.3838(3) 0.6429(3) 0.5049(3) 0.0447(7) Uani 1 1 d . . .
H14A H 0.4029 0.7326 0.4908 0.054 Uiso 1 1 calc R . .
H14B H 0.4882 0.6297 0.5419 0.054 Uiso 1 1 calc R . .
C15 C 0.2691(3) 0.5273(2) 0.3897(2) 0.0378(6) Uani 1 1 d . . .
H15A H 0.1938 0.5594 0.3333 0.045 Uiso 1 1 calc R . .
H15B H 0.3288 0.4888 0.3511 0.045 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N1 175.20(8) . 2_556 ?
N2 Cu1 Cu2 133.52(6) . 2_556 ?
N1 Cu1 Cu2 44.58(5) 2_556 2_556 ?
N2 Cu1 Cu2 42.54(6) . . ?
N1 Cu1 Cu2 135.21(5) 2_556 . ?
Cu2 Cu1 Cu2 90.975(18) 2_556 . ?
N2 Cu2 N1 174.10(8) . . ?
N2 Cu2 Cu1 131.72(6) . 2_556 ?
N1 Cu2 Cu1 44.70(5) . 2_556 ?
N2 Cu2 Cu1 42.70(6) . . ?
N1 Cu2 Cu1 133.39(6) . . ?
Cu1 Cu2 Cu1 89.024(19) 2_556 . ?
Si2 N1 Si1 125.09(10) . . ?
Si2 N1 Cu2 110.70(9) . . ?
Si1 N1 Cu2 107.65(9) . . ?
Si2 N1 Cu1 110.83(9) . 2_556 ?
Si1 N1 Cu1 106.38(9) . 2_556 ?
Cu2 N1 Cu1 90.72(7) . 2_556 ?
C7 N2 Cu2 133.99(16) . . ?
C7 N2 Cu1 131.22(16) . . ?
Cu2 N2 Cu1 94.76(8) . . ?
C7 N3 C10 116.61(18) . . ?
C7 N3 C8 114.26(19) . . ?
C10 N3 C8 113.25(19) . . ?
C7 N4 C12 122.38(19) . . ?
C7 N4 C15 124.2(2) . . ?
C12 N4 C15 111.4(2) . . ?
N1 Si1 C2 112.05(11) . . ?
N1 Si1 C1 109.82(11) . . ?
C2 Si1 C1 107.17(15) . . ?
N1 Si1 C3 111.22(12) . . ?
C2 Si1 C3 108.92(18) . . ?
C1 Si1 C3 107.48(13) . . ?
N1 Si1 Cu1 38.73(6) . 2_556 ?
C2 Si1 Cu1 91.47(12) . 2_556 ?
C1 Si1 Cu1 86.50(9) . 2_556 ?
C3 Si1 Cu1 149.72(10) . 2_556 ?
N1 Si2 C4 109.18(10) . . ?
N1 Si2 C6 112.03(11) . . ?
C4 Si2 C6 109.35(12) . . ?
N1 Si2 C5 112.83(10) . . ?
C4 Si2 C5 107.11(12) . . ?
C6 Si2 C5 106.16(11) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 N4 124.2(2) . . ?
N2 C7 N3 125.1(2) . . ?
N4 C7 N3 110.63(19) . . ?
N3 C8 C9 112.3(2) . . ?
N3 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N3 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 C11 112.2(2) . . ?
N3 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
N3 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 C13 103.7(2) . . ?
N4 C12 H12A 111.0 . . ?
C13 C12 H12A 111.0 . . ?
N4 C12 H12B 111.0 . . ?
C13 C12 H12B 111.0 . . ?
H12A C12 H12B 109.0 . . ?
C12 C13 C14 102.4(2) . . ?
C12 C13 H13A 111.3 . . ?
C14 C13 H13A 111.3 . . ?
C12 C13 H13B 111.3 . . ?
C14 C13 H13B 111.3 . . ?
H13A C13 H13B 109.2 . . ?
C15 C14 C13 103.1(2) . . ?
C15 C14 H14A 111.1 . . ?
C13 C14 H14A 111.1 . . ?
C15 C14 H14B 111.1 . . ?
C13 C14 H14B 111.1 . . ?
H14A C14 H14B 109.1 . . ?
N4 C15 C14 103.6(2) . . ?
N4 C15 H15A 111.0 . . ?
C14 C15 H15A 111.0 . . ?
N4 C15 H15B 111.0 . . ?
C14 C15 H15B 111.0 . . ?
H15A C15 H15B 109.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.8544(19) . ?
Cu1 N1 1.9137(18) 2_556 ?
Cu1 Cu2 2.7204(5) 2_556 ?
Cu1 Cu2 2.7252(6) . ?
Cu2 N2 1.8490(18) . ?
Cu2 N1 1.9096(18) . ?
Cu2 Cu1 2.7204(5) 2_556 ?
N1 Si2 1.7418(18) . ?
N1 Si1 1.7495(18) . ?
N1 Cu1 1.9137(18) 2_556 ?
N2 C7 1.279(3) . ?
N3 C7 1.427(3) . ?
N3 C10 1.455(3) . ?
N3 C8 1.474(3) . ?
N4 C7 1.375(3) . ?
N4 C12 1.446(3) . ?
N4 C15 1.478(3) . ?
Si1 C2 1.865(3) . ?
Si1 C1 1.866(3) . ?
Si1 C3 1.867(3) . ?
Si2 C4 1.869(2) . ?
Si2 C6 1.880(3) . ?
Si2 C5 1.880(3) . ?
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 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 C9 1.516(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.518(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.520(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.527(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.520(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
