#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/31/7103135.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_7103135
loop_
_publ_author_name
'Donnelly, Paul S'
'Zanatta, Shannon D'
'Zammit, Steven C'
'White, Jonathan M'
'Williams, Spencer J'
_publ_section_title
;
 'Click' cycloaddition catalysts: copper(I) and copper(II)
 tris(triazolylmethyl)amine complexes.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2459
_journal_page_last               2461
_journal_paper_doi               10.1039/b719724a
_journal_year                    2008
_chemical_formula_sum            'C10 H8 Cl0.5 Cu0.33 N3.33'
_chemical_formula_weight         213.77
_chemical_name_common            'Cu(ii) complex with TBTA'
_chemical_name_systematic
;
?
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -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            24
_cell_length_a                   17.6375(2)
_cell_length_b                   17.6375(2)
_cell_length_c                   17.6375(2)
_cell_measurement_reflns_used    1080
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.1262
_cell_measurement_theta_min      3.5486
_cell_volume                     5486.70(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.0711
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Oxford Xcalibur'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8136
_diffrn_reflns_theta_full        64.87
_diffrn_reflns_theta_max         64.87
_diffrn_reflns_theta_min         4.34
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1969
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1783P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2532
_refine_ls_wR_factor_ref         0.3260
_reflns_number_gt                575
_reflns_number_total             1524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719724a.txt
_cod_data_source_block           pdsw
_cod_original_sg_symbol_H-M      'I 21/a -3'
_cod_original_formula_sum        'C10 H8 Cl0.50 Cu0.33 N3.33'
_cod_database_code               7103135
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5993(7) 0.1786(8) 0.2940(9) 0.108(5) Uani 1 1 d . . .
H1A H 0.5639 0.1633 0.3333 0.129 Uiso 1 1 calc R . .
H1B H 0.5937 0.1448 0.2510 0.129 Uiso 1 1 calc R . .
C2 C 0.5850(7) 0.2624(8) 0.2700(8) 0.099(4) Uani 1 1 d . . .
C3 C 0.5192(6) 0.3018(8) 0.2549(7) 0.084(4) Uani 1 1 d . . .
H3 H 0.4698 0.2887 0.2677 0.101 Uiso 1 1 calc R . .
C4 C 0.4954(6) 0.4249(6) 0.1910(9) 0.100(5) Uani 1 1 d . . .
H4A H 0.4428 0.4087 0.1908 0.120 Uiso 1 1 calc R . .
H4B H 0.5095 0.4369 0.1392 0.120 Uiso 1 1 calc R . .
C5 C 0.5026(7) 0.4937(8) 0.2379(12) 0.107(6) Uani 1 1 d . . .
C6 C 0.5461(7) 0.5537(9) 0.2180(12) 0.133(7) Uani 1 1 d . . .
H6 H 0.5694 0.5540 0.1707 0.160 Uiso 1 1 calc R . .
C7 C 0.5574(10) 0.6184(9) 0.2691(16) 0.176(11) Uani 1 1 d . . .
H7 H 0.5904 0.6575 0.2565 0.212 Uiso 1 1 calc R . .
C8 C 0.5170(12) 0.6193(11) 0.3373(19) 0.183(11) Uani 1 1 d . . .
H8 H 0.5197 0.6602 0.3704 0.219 Uiso 1 1 calc R . .
C9 C 0.4706(13) 0.5529(15) 0.3538(16) 0.186(9) Uani 1 1 d . . .
H9 H 0.4441 0.5521 0.3993 0.224 Uiso 1 1 calc R . .
C10 C 0.4639(12) 0.4934(9) 0.3077(16) 0.144(8) Uani 1 1 d . . .
H10 H 0.4339 0.4523 0.3215 0.172 Uiso 1 1 calc R . .
N1 N 0.6435(4) 0.3020(5) 0.2406(5) 0.059(2) Uani 1 1 d . . .
N3 N 0.5429(5) 0.3623(5) 0.2183(6) 0.076(3) Uani 1 1 d . . .
N2 N 0.6183(5) 0.3618(5) 0.2085(6) 0.076(3) Uani 1 1 d . . .
N4 N 0.6774(4) 0.1774(4) 0.3226(4) 0.045(3) Uani 1 3 d S . .
Cl1 Cl 0.81990(15) 0.31990(15) 0.18010(15) 0.0724(13) Uani 1 3 d S . .
Cu1 Cu 0.74678(7) 0.24678(7) 0.25322(7) 0.0548(8) Uani 1 3 d S . .
Cl2 Cl 0.0417(3) 0.0417(3) 0.0417(3) 0.074(2) Uani 0.50 3 d SP . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
N4 C1 C2 105.0(10) . . ?
N1 C2 C3 107.9(11) . . ?
N1 C2 C1 118.2(10) . . ?
C3 C2 C1 131.8(13) . . ?
N3 C3 C2 103.7(10) . . ?
N3 C4 C5 112.7(11) . . ?
C6 C5 C10 120.3(17) . . ?
C6 C5 C4 123.2(18) . . ?
C10 C5 C4 116.4(14) . . ?
C5 C6 C7 121.7(18) . . ?
C8 C7 C6 117.9(18) . . ?
C7 C8 C9 117(2) . . ?
C10 C9 C8 124(3) . . ?
C9 C10 C5 119(2) . . ?
N2 N1 C2 109.4(9) . . ?
N2 N1 Cu1 137.7(7) . . ?
C2 N1 Cu1 112.7(7) . . ?
C3 N3 N2 111.9(9) . . ?
C3 N3 C4 126.2(10) . . ?
N2 N3 C4 121.9(10) . . ?
N1 N2 N3 107.0(9) . . ?
C1 N4 C1 109.4(7) 8_645 . ?
C1 N4 C1 109.4(7) 8_645 11_556 ?
C1 N4 C1 109.4(7) . 11_556 ?
C1 N4 Cu1 109.6(7) 8_645 . ?
C1 N4 Cu1 109.6(7) . . ?
C1 N4 Cu1 109.6(7) 11_556 . ?
N1 Cu1 N1 117.03(14) 8_645 . ?
N1 Cu1 N1 117.03(14) 8_645 11_556 ?
N1 Cu1 N1 117.03(14) . 11_556 ?
N1 Cu1 N4 80.0(2) 8_645 . ?
N1 Cu1 N4 80.0(2) . . ?
N1 Cu1 N4 80.0(2) 11_556 . ?
N1 Cu1 Cl1 100.0(2) 8_645 . ?
N1 Cu1 Cl1 100.0(2) . . ?
N1 Cu1 Cl1 100.0(2) 11_556 . ?
N4 Cu1 Cl1 180.0(4) . . ?
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
C1 N4 1.467(13) . ?
C1 C2 1.557(17) . ?
C2 N1 1.349(15) . ?
C2 C3 1.379(15) . ?
C3 N3 1.315(15) . ?
C4 N3 1.467(13) . ?
C4 C5 1.48(2) . ?
C5 C6 1.353(18) . ?
C5 C10 1.41(3) . ?
C6 C7 1.47(2) . ?
C7 C8 1.40(3) . ?
C8 C9 1.46(3) . ?
C9 C10 1.33(3) . ?
N1 N2 1.278(11) . ?
N1 Cu1 2.078(7) . ?
N3 N2 1.341(13) . ?
N4 C1 1.467(13) 8_645 ?
N4 C1 1.467(13) 11_556 ?
N4 Cu1 2.120(11) . ?
Cl1 Cu1 2.233(5) . ?
Cu1 N1 2.078(7) 8_645 ?
Cu1 N1 2.078(7) 11_556 ?
