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#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008596.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_7008596
loop_
_publ_author_name
'Bond, Andrew D.'
'Derossi, Sofia'
'Harding, Charles J.'
'McInnes, Eric J. L.'
'McKee, Vickie'
'McKenzie, Christine J.'
'Nelson, Jane'
'Wolowska, Joanna'
_publ_section_title
;
 Cascade complexation: a single cyano bridge links a pair of Cu(II)
 cations.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2403
_journal_page_last               2409
_journal_paper_doi               10.1039/b504916d
_journal_year                    2005
_chemical_formula_moiety         'C37 H54 Cu2 N9, 3(Cl O4)'
_chemical_formula_sum            'C37 H54 Cl3 Cu2 N9 O12'
_chemical_formula_weight         1050.32
_chemical_name_common            '[Cu₂(CN)L²](ClO₄)₃'
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.385(2)
_cell_length_b                   10.385(2)
_cell_length_c                   24.107(7)
_cell_measurement_reflns_used    1433
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.42
_cell_volume                     2251.6(9)
_computing_cell_refinement       'SAINT v.7.06a (Bruker, 2003)'
_computing_data_collection       'APEX2 v.1.0-8 (Bruker-Nonius, 2003)'
_computing_data_reduction        'SAINT v.7.06a (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL v.6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL v.6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice ω and 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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10659
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Sheldrick, 2003)
Ratio of minimum to maximum apparent transmission: 0.744432
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1468
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0720P)²+5.6209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                988
_reflns_number_total             1468
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b504916d.txt
_cod_data_source_block           3
_cod_database_code               7008596
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.6667 0.3333 0.14460(4) 0.0277(3) Uani 1 3 d S . .
N1 N 0.6667 0.3333 0.0590(3) 0.0297(15) Uani 1 3 d S . .
N2 N 0.4730(4) 0.3540(4) 0.13530(15) 0.0290(9) Uani 1 1 d . . .
H2 H 0.4846 0.4286 0.1596 0.035 Uiso 1 1 calc R . .
C1 C 0.5268(6) 0.3258(6) 0.0395(2) 0.0378(13) Uani 1 1 d . . .
H1A H 0.4456 0.2208 0.0384 0.045 Uiso 1 1 calc R . .
H1B H 0.5410 0.3671 0.0016 0.045 Uiso 1 1 calc R . .
C2 C 0.4853(6) 0.4142(6) 0.0787(2) 0.0370(12) Uani 1 1 d . . .
H2A H 0.5625 0.5207 0.0778 0.044 Uiso 1 1 calc R . .
H2B H 0.3894 0.4048 0.0674 0.044 Uiso 1 1 calc R . .
C3 C 0.3201(5) 0.2248(5) 0.14535(19) 0.0314(11) Uani 1 1 d . . .
H3A H 0.2933 0.1522 0.1147 0.038 Uiso 1 1 calc R . .
H3B H 0.2476 0.2602 0.1455 0.038 Uiso 1 1 calc R . .
C4 C 0.3110(5) 0.1492(5) 0.19959(19) 0.0280(11) Uani 1 1 d . . .
C5 C 0.3065(5) 0.0135(5) 0.2003(2) 0.0297(11) Uani 1 1 d . . .
H5A H 0.3045 -0.0333 0.1662 0.036 Uiso 1 1 calc R . .
C6 C 0.3051(8) -0.0554(8) 0.2500 0.0332(16) Uani 1 2 d S . .
H6A H 0.3031 -0.1478 0.2500 0.040 Uiso 1 2 calc SR . .
C7 C 0.3116(7) 0.2156(8) 0.2500 0.0302(15) Uani 1 2 d S . .
H7A H 0.3125 0.3075 0.2500 0.036 Uiso 1 2 calc SR . .
N100 N 0.6667 0.3333 0.2262(3) 0.0266(16) Uani 0.50 3 d SP . .
C100 C 0.6667 0.3333 0.2262(3) 0.0266(16) Uani 0.50 3 d SP . .
Cl1 Cl 0.3333 0.6667 0.14183(10) 0.0418(6) Uani 1 3 d SD . .
O1A O 0.3333 0.6667 0.0842(2) 0.156(6) Uani 1 3 d SD . .
O1B O 0.3408(5) 0.5426(4) 0.16275(18) 0.0693(14) Uani 1 1 d D . .
Cl2 Cl 0.0394(14) 0.1109(11) 0.0066(5) 0.076(3) Uiso 0.17 1 d PD A -1
O2A O 0.025(5) 0.004(3) 0.0461(7) 0.088(10) Uiso 0.17 1 d PD A -1
O2B O 0.0350(19) 0.2296(15) 0.0337(7) 0.108(6) Uiso 0.33 1 d PD A -1
O2C O 0.176(2) 0.167(3) -0.0216(14) 0.055(13) Uiso 0.08 1 d PD A -1
O2D O -0.079(3) 0.044(3) -0.0318(11) 0.066(16) Uiso 0.08 1 d PD A -1
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'
O O 0.0106 0.0060 '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'
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
N100 Cu1 N1 180.000(1) . . ?
N100 Cu1 N2 96.02(10) . 3_665 ?
N1 Cu1 N2 83.98(10) . 3_665 ?
N100 Cu1 N2 96.02(10) . . ?
N1 Cu1 N2 83.98(10) . . ?
N2 Cu1 N2 118.91(4) 3_665 . ?
N100 Cu1 N2 96.02(10) . 2_655 ?
N1 Cu1 N2 83.98(10) . 2_655 ?
N2 Cu1 N2 118.92(4) 3_665 2_655 ?
N2 Cu1 N2 118.91(4) . 2_655 ?
C1 N1 C1 110.6(3) 2_655 . ?
C1 N1 C1 110.6(3) 2_655 3_665 ?
C1 N1 C1 110.6(3) . 3_665 ?
C1 N1 Cu1 108.4(3) 2_655 . ?
C1 N1 Cu1 108.4(3) . . ?
C1 N1 Cu1 108.4(3) 3_665 . ?
C2 N2 C3 110.8(4) . . ?
C2 N2 Cu1 104.6(3) . . ?
C3 N2 Cu1 121.4(3) . . ?
C2 N2 H2 106.3 . . ?
C3 N2 H2 106.3 . . ?
Cu1 N2 H2 106.3 . . ?
N1 C1 C2 109.5(4) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 108.0(4) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 111.7(4) . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C7 118.7(5) . . ?
C5 C4 C3 120.2(4) . . ?
C7 C4 C3 121.1(4) . . ?
C4 C5 C6 121.3(5) . . ?
C4 C5 H5A 119.3 . . ?
C6 C5 H5A 119.3 . . ?
C5 C6 C5 118.8(6) 10_556 . ?
C5 C6 H6A 120.6 10_556 . ?
C5 C6 H6A 120.6 . . ?
C4 C7 C4 121.1(6) 10_556 . ?
C4 C7 H7A 119.4 10_556 . ?
C4 C7 H7A 119.4 . . ?
C100 N100 Cu1 179.998(1) 10_556 . ?
O1A Cl1 O1B 110.78(17) . 3_565 ?
O1A Cl1 O1B 110.78(17) . 2_665 ?
O1B Cl1 O1B 108.13(18) 3_565 2_665 ?
O1A Cl1 O1B 110.78(17) . . ?
O1B Cl1 O1B 108.13(18) 3_565 . ?
O1B Cl1 O1B 108.13(18) 2_665 . ?
O2A Cl2 O2C 109.6(4) . . ?
O2A Cl2 O2D 109.5(4) . . ?
O2C Cl2 O2D 109.6(4) . . ?
O2A Cl2 O2B 109.6(4) . . ?
O2C Cl2 O2B 109.3(4) . . ?
O2D Cl2 O2B 109.3(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
Cu1 N100 1.967(7) . ?
Cu1 N1 2.064(7) . ?
Cu1 N2 2.138(4) 3_665 ?
Cu1 N2 2.138(4) . ?
Cu1 N2 2.138(4) 2_655 ?
N1 C1 1.491(5) 2_655 ?
N1 C1 1.491(5) . ?
N1 C1 1.491(5) 3_665 ?
N2 C2 1.478(6) . ?
N2 C3 1.500(6) . ?
N2 H2 0.9300 . ?
C1 C2 1.523(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.504(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.387(6) . ?
C4 C7 1.395(6) . ?
C5 C6 1.391(6) . ?
C5 H5A 0.9500 . ?
C6 C5 1.391(6) 10_556 ?
C6 H6A 0.9500 . ?
C7 C4 1.395(6) 10_556 ?
C7 H7A 0.9500 . ?
N100 C100 1.149(14) 10_556 ?
Cl1 O1A 1.389(6) . ?
Cl1 O1B 1.421(4) 3_565 ?
Cl1 O1B 1.421(4) 2_665 ?
Cl1 O1B 1.421(4) . ?
Cl2 O2A 1.411(6) . ?
Cl2 O2C 1.412(6) . ?
Cl2 O2D 1.412(6) . ?
Cl2 O2B 1.416(6) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Cu1 N1 C1 112.2(2) 3_665 . . 2_655 ?
N2 Cu1 N1 C1 -127.8(2) . . . 2_655 ?
N2 Cu1 N1 C1 -7.8(2) 2_655 . . 2_655 ?
N2 Cu1 N1 C1 -127.8(2) 3_665 . . . ?
N2 Cu1 N1 C1 -7.8(2) . . . . ?
N2 Cu1 N1 C1 112.2(2) 2_655 . . . ?
N2 Cu1 N1 C1 -7.8(2) 3_665 . . 3_665 ?
N2 Cu1 N1 C1 112.2(2) . . . 3_665 ?
N2 Cu1 N1 C1 -127.8(2) 2_655 . . 3_665 ?
N100 Cu1 N2 C2 158.6(3) . . . . ?
N1 Cu1 N2 C2 -21.4(3) . . . . ?
N2 Cu1 N2 C2 58.3(4) 3_665 . . . ?
N2 Cu1 N2 C2 -101.1(3) 2_655 . . . ?
N100 Cu1 N2 C3 -75.3(3) . . . . ?
N1 Cu1 N2 C3 104.7(3) . . . . ?
N2 Cu1 N2 C3 -175.5(2) 3_665 . . . ?
N2 Cu1 N2 C3 25.0(4) 2_655 . . . ?
C1 N1 C1 C2 154.3(5) 2_655 . . . ?
C1 N1 C1 C2 -82.9(6) 3_665 . . . ?
Cu1 N1 C1 C2 35.7(4) . . . . ?
C3 N2 C2 C1 -86.3(5) . . . . ?
Cu1 N2 C2 C1 46.2(4) . . . . ?
N1 C1 C2 N2 -56.4(5) . . . . ?
C2 N2 C3 C4 172.4(4) . . . . ?
Cu1 N2 C3 C4 49.1(5) . . . . ?
N2 C3 C4 C5 -105.0(5) . . . . ?
N2 C3 C4 C7 72.9(6) . . . . ?
C7 C4 C5 C6 -1.0(7) . . . . ?
C3 C4 C5 C6 177.0(5) . . . . ?
C4 C5 C6 C5 0.7(9) . . . 10_556 ?
C5 C4 C7 C4 1.3(9) . . . 10_556 ?
C3 C4 C7 C4 -176.6(4) . . . 10_556 ?
