#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/14/4311430.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_4311430
loop_
_publ_author_name
'Sarah H. Oakley'
'Martyn P. Coles'
'Peter B. Hitchcock'
_publ_section_title
;
 Structural Consequences of the Prohibition of Hydrogen Bonding in
 Copper-Guanidine Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5168
_journal_page_last               5172
_journal_paper_doi               10.1021/ic0495970
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C10 H21 Cl1 Cu1 N3 Si1'
_chemical_formula_sum            'C10 H21 Cl Cu N3 Si'
_chemical_formula_weight         310.38
_chemical_name_common            '[CuCl(C7H12N2SiMe3]'
_chemical_name_systematic
;
 ?
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-02-27T17:38:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                111.982(3)
_cell_angle_beta                 97.576(3)
_cell_angle_gamma                106.227(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8072(3)
_cell_length_b                   9.6668(3)
_cell_length_c                   10.7091(5)
_cell_measurement_reflns_used    4337
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     693.77(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5274
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  0.8109
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.6894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.067
_reflns_number_gt                2071
_reflns_number_total             2349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495970si20040326_052428_3.cif
_cod_data_source_block           (3)-feb2903
_cod_original_formula_sum        'C10 H21 Cl1 Cu1 N3 Si1'
_cod_database_code               4311430
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
Cu Cu 0.69167(4) 0.35177(4) 0.32681(3) 0.02425(12) Uani 1 1 d . . .
Cl Cl 0.75352(10) 0.14905(8) 0.31233(7) 0.03008(17) Uani 1 1 d . . .
Si Si 0.33669(10) 0.25470(8) 0.06232(7) 0.02109(17) Uani 1 1 d . . .
N1 N 0.6518(3) 0.5389(2) 0.3401(2) 0.0219(5) Uani 1 1 d . . .
N2 N 0.3411(3) 0.4115(2) 0.2188(2) 0.0214(5) Uani 1 1 d . . .
N3 N 0.4567(3) 0.6873(2) 0.3588(2) 0.0218(5) Uani 1 1 d . . .
C1 C 0.4885(3) 0.5483(3) 0.3069(3) 0.0190(5) Uani 1 1 d . . .
C2 C 0.8090(4) 0.6906(3) 0.4215(3) 0.0264(6) Uani 1 1 d . . .
H2A H 0.851(4) 0.740(3) 0.362(3) 0.030(8) Uiso 1 1 d . . .
H2B H 0.913(4) 0.667(3) 0.457(3) 0.024(7) Uiso 1 1 d . . .
C3 C 0.7536(4) 0.8030(3) 0.5364(3) 0.0276(6) Uani 1 1 d . . .
H3A H 0.718(4) 0.756(3) 0.597(3) 0.026(7) Uiso 1 1 d . . .
H3B H 0.856(4) 0.900(4) 0.591(3) 0.037(8) Uiso 1 1 d . . .
C4 C 0.5959(4) 0.8349(3) 0.4693(3) 0.0281(6) Uani 1 1 d . . .
H4A H 0.535(4) 0.881(3) 0.538(3) 0.030(8) Uiso 1 1 d . . .
H4B H 0.641(4) 0.905(4) 0.431(3) 0.030(8) Uiso 1 1 d . . .
C5 C 0.2836(4) 0.7080(3) 0.3112(3) 0.0264(6) Uani 1 1 d . . .
H5A H 0.314(4) 0.786(3) 0.273(3) 0.019(7) Uiso 1 1 d . . .
H5B H 0.246(4) 0.753(4) 0.396(3) 0.038(8) Uiso 1 1 d . . .
C6 C 0.1320(4) 0.5537(4) 0.2088(3) 0.0293(6) Uani 1 1 d . . .
H6A H 0.143(4) 0.535(3) 0.117(3) 0.020(7) Uiso 1 1 d . . .
H6B H 0.020(5) 0.559(3) 0.216(3) 0.034(8) Uiso 1 1 d . . .
C7 C 0.1593(4) 0.4191(4) 0.2382(3) 0.0269(6) Uani 1 1 d . . .
H7A H 0.159(4) 0.443(3) 0.335(3) 0.033(8) Uiso 1 1 d . . .
H7B H 0.061(4) 0.316(4) 0.177(3) 0.028(7) Uiso 1 1 d . . .
C8 C 0.1573(5) 0.2364(4) -0.0828(3) 0.0310(7) Uani 1 1 d . . .
H8A H 0.203(5) 0.329(4) -0.103(4) 0.056(10) Uiso 1 1 d . . .
H8B H 0.041(5) 0.226(4) -0.064(3) 0.042(9) Uiso 1 1 d . . .
H8C H 0.148(4) 0.147(4) -0.160(3) 0.036(8) Uiso 1 1 d . . .
C9 C 0.2684(5) 0.0669(3) 0.0831(3) 0.0298(6) Uani 1 1 d . . .
H9A H 0.152(5) 0.047(4) 0.112(4) 0.056(10) Uiso 1 1 d . . .
H9B H 0.365(5) 0.067(4) 0.146(3) 0.037(8) Uiso 1 1 d . . .
H9C H 0.245(5) -0.018(4) -0.003(4) 0.051(10) Uiso 1 1 d . . .
C10 C 0.5562(4) 0.2967(4) 0.0104(3) 0.0318(7) Uani 1 1 d . . .
H10A H 0.588(6) 0.392(5) 0.003(4) 0.071(13) Uiso 1 1 d . . .
H10B H 0.526(5) 0.216(4) -0.084(4) 0.056(10) Uiso 1 1 d . . .
H10C H 0.657(5) 0.292(4) 0.064(4) 0.053(11) Uiso 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'
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'
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'
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
N1 Cu Cl 176.43(7) . . ?
N2 Si C9 108.15(12) . . ?
N2 Si C10 113.26(12) . . ?
C9 Si C10 113.08(16) . . ?
N2 Si C8 107.81(12) . . ?
C9 Si C8 109.00(14) . . ?
C10 Si C8 105.33(16) . . ?
C1 N1 C2 117.0(2) . . ?
C1 N1 Cu 124.78(17) . . ?
C2 N1 Cu 116.80(17) . . ?
C1 N2 C7 113.9(2) . . ?
C1 N2 Si 127.87(16) . . ?
C7 N2 Si 116.17(18) . . ?
C1 N3 C4 122.3(2) . . ?
C1 N3 C5 124.8(2) . . ?
C4 N3 C5 112.9(2) . . ?
N1 C1 N3 122.9(2) . . ?
N1 C1 N2 119.2(2) . . ?
N3 C1 N2 117.9(2) . . ?
N1 C2 C3 110.0(2) . . ?
N1 C2 H2A 110.8(17) . . ?
C3 C2 H2A 109.9(16) . . ?
N1 C2 H2B 108.4(16) . . ?
C3 C2 H2B 112.3(16) . . ?
H2A C2 H2B 105(2) . . ?
C4 C3 C2 108.0(2) . . ?
C4 C3 H3A 111.1(17) . . ?
C2 C3 H3A 109.5(17) . . ?
C4 C3 H3B 110.5(18) . . ?
C2 C3 H3B 110.2(18) . . ?
H3A C3 H3B 108(3) . . ?
N3 C4 C3 111.5(2) . . ?
N3 C4 H4A 107.3(17) . . ?
C3 C4 H4A 110.2(18) . . ?
N3 C4 H4B 108.8(19) . . ?
C3 C4 H4B 109.8(18) . . ?
H4A C4 H4B 109(2) . . ?
N3 C5 C6 113.5(2) . . ?
N3 C5 H5A 107.6(15) . . ?
C6 C5 H5A 112.1(16) . . ?
N3 C5 H5B 104.3(19) . . ?
C6 C5 H5B 109.4(19) . . ?
H5A C5 H5B 110(2) . . ?
C5 C6 C7 108.5(2) . . ?
C5 C6 H6A 108.6(16) . . ?
C7 C6 H6A 108.1(15) . . ?
C5 C6 H6B 110.7(19) . . ?
C7 C6 H6B 111(2) . . ?
H6A C6 H6B 110(3) . . ?
N2 C7 C6 108.5(2) . . ?
N2 C7 H7A 109.4(18) . . ?
C6 C7 H7A 108.1(17) . . ?
N2 C7 H7B 109.9(16) . . ?
C6 C7 H7B 112.2(17) . . ?
H7A C7 H7B 109(2) . . ?
Si C8 H8A 109(2) . . ?
Si C8 H8B 114(2) . . ?
H8A C8 H8B 111(3) . . ?
Si C8 H8C 106(2) . . ?
H8A C8 H8C 107(3) . . ?
H8B C8 H8C 110(3) . . ?
Si C9 H9A 112(2) . . ?
Si C9 H9B 110.5(19) . . ?
H9A C9 H9B 111(3) . . ?
Si C9 H9C 109(2) . . ?
H9A C9 H9C 106(3) . . ?
H9B C9 H9C 108(3) . . ?
Si C10 H10A 111(2) . . ?
Si C10 H10B 104(2) . . ?
H10A C10 H10B 105(3) . . ?
Si C10 H10C 117(2) . . ?
H10A C10 H10C 110(3) . . ?
H10B C10 H10C 109(3) . . ?
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
Cu N1 1.877(2) . ?
Cu Cl 2.1022(7) . ?
Si N2 1.778(2) . ?
Si C9 1.850(3) . ?
Si C10 1.856(3) . ?
Si C8 1.868(3) . ?
N1 C1 1.315(3) . ?
N1 C2 1.474(3) . ?
N2 C1 1.376(3) . ?
N2 C7 1.479(3) . ?
N3 C1 1.356(3) . ?
N3 C4 1.465(3) . ?
N3 C5 1.474(3) . ?
C2 C3 1.511(4) . ?
C2 H2A 0.97(3) . ?
C2 H2B 0.97(3) . ?
C3 C4 1.508(4) . ?
C3 H3A 0.94(3) . ?
C3 H3B 0.95(3) . ?
C4 H4A 0.97(3) . ?
C4 H4B 0.94(3) . ?
C5 C6 1.508(4) . ?
C5 H5A 0.98(3) . ?
C5 H5B 0.97(3) . ?
C6 C7 1.511(4) . ?
C6 H6A 0.95(3) . ?
C6 H6B 0.90(3) . ?
C7 H7A 0.97(3) . ?
C7 H7B 0.98(3) . ?
C8 H8A 0.98(4) . ?
C8 H8B 0.94(3) . ?
C8 H8C 0.92(3) . ?
C9 H9A 0.99(4) . ?
C9 H9B 0.94(3) . ?
C9 H9C 0.93(4) . ?
C10 H10A 0.92(4) . ?
C10 H10B 0.97(4) . ?
C10 H10C 0.93(4) . ?
