#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/86/4328629.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_4328629
loop_
_publ_author_name
'Pampa M. Guha'
'Hoa Phan'
'Jared S. Kinyon'
'Wendy S. Brotherton'
'Kesavapillai Sreenath'
'J. Tyler Simmons'
'Zhenxing Wang'
'Ronald J. Clark'
'Naresh S. Dalal'
'Michael Shatruk'
'Lei Zhu'
_publ_section_title
;
 Structurally Diverse Copper(II) Complexes of Polyaza Ligands Containing
 1,2,3-Triazoles: Site Selectivity and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3465
_journal_page_last               3477
_journal_paper_doi               10.1021/ic2021319
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C28 H24 Cl2 Cu N16 O8'
_chemical_formula_sum            'C28 H24 Cl2 Cu N16 O8'
_chemical_formula_weight         847.07
_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                98.4470(10)
_cell_angle_beta                 92.9640(10)
_cell_angle_gamma                114.8660(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3590(6)
_cell_length_b                   8.3744(6)
_cell_length_c                   13.3450(13)
_cell_measurement_reflns_used    6880
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.71
_cell_volume                     831.64(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9248
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             431
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0268
_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)+(0.0340P)²+0.5475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                3490
_reflns_number_total             3647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2021319_si_001_4.cif
_cod_data_source_block           complex4
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4328629
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
Cu1 Cu 0.5000 0.0000 0.0000 0.02039(8) Uani 1 2 d S
C1 C 0.4105(2) 0.2671(2) -0.09439(11) 0.0270(3) Uani 1 1 d .
H1 H 0.4970 0.2714 -0.1387 0.032 Uiso 1 1 calc R
C2 C 0.3184(2) 0.3690(2) -0.10482(12) 0.0303(3) Uani 1 1 d .
H2 H 0.3427 0.4431 -0.1549 0.036 Uiso 1 1 calc R
C3 C 0.1907(2) 0.3617(2) -0.04148(13) 0.0320(4) Uani 1 1 d .
H3 H 0.1240 0.4284 -0.0486 0.038 Uiso 1 1 calc R
C4 C 0.1611(2) 0.2559(2) 0.03267(12) 0.0293(3) Uani 1 1 d .
H4 H 0.0748 0.2494 0.0775 0.035 Uiso 1 1 calc R
C5 C 0.2605(2) 0.1600(2) 0.03986(11) 0.0231(3) Uani 1 1 d .
C6 C 0.2495(2) 0.05185(19) 0.11806(11) 0.0225(3) Uani 1 1 d .
C7 C 0.1630(2) 0.0239(2) 0.20259(11) 0.0254(3) Uani 1 1 d .
H7 H 0.0799 0.0669 0.2250 0.030 Uiso 1 1 calc R
C8 C 0.1781(2) -0.1494(2) 0.34123(12) 0.0299(3) Uani 1 1 d .
H8A H 0.2438 -0.2212 0.3524 0.036 Uiso 1 1 calc R
H8B H 0.0495 -0.2303 0.3329 0.036 Uiso 1 1 calc R
C9 C 0.2218(2) -0.0046(2) 0.43430(11) 0.0238(3) Uani 1 1 d .
C10 C 0.2918(2) -0.0200(2) 0.52719(13) 0.0291(3) Uani 1 1 d .
H10 H 0.3215 -0.1164 0.5324 0.035 Uiso 1 1 calc R
C11 C 0.3168(2) 0.1090(2) 0.61181(13) 0.0342(4) Uani 1 1 d .
H11 H 0.3633 0.1020 0.6767 0.041 Uiso 1 1 calc R
C12 C 0.2736(2) 0.2483(2) 0.60097(12) 0.0318(3) Uani 1 1 d .
H12 H 0.2908 0.3389 0.6580 0.038 Uiso 1 1 calc R
C13 C 0.2045(2) 0.2532(2) 0.50529(12) 0.0264(3) Uani 1 1 d .
N15 N 0.17748(18) 0.12818(17) 0.42278(10) 0.0252(3) Uani 1 1 d .
C15 C 0.1516(2) 0.3992(2) 0.48722(13) 0.0339(4) Uani 1 1 d .
H15A H 0.0365 0.3450 0.4427 0.041 Uiso 1 1 calc R
H15B H 0.1352 0.4580 0.5533 0.041 Uiso 1 1 calc R
N1 N 0.38172(17) 0.16242(16) -0.02375(9) 0.0215(2) Uani 1 1 d .
N2 N 0.35359(17) -0.03645(16) 0.11526(9) 0.0221(2) Uani 1 1 d .
N3 N 0.33849(18) -0.11658(17) 0.19404(10) 0.0253(3) Uani 1 1 d .
N4 N 0.22279(18) -0.07896(17) 0.24687(9) 0.0247(3) Uani 1 1 d .
N5 N 0.2858(2) 0.5358(2) 0.43906(12) 0.0395(4) Uani 1 1 d .
N6 N 0.3063(2) 0.48230(19) 0.35106(12) 0.0341(3) Uani 1 1 d .
N7 N 0.3417(2) 0.4570(2) 0.27156(13) 0.0460(4) Uani 1 1 d .
Cl1 Cl 0.80237(5) 0.29215(5) 0.21400(3) 0.02938(10) Uani 1 1 d .
O1 O 0.74662(18) 0.25759(16) 0.10531(9) 0.0393(3) Uani 1 1 d .
O2 O 0.8587(2) 0.1610(2) 0.23507(13) 0.0562(4) Uani 1 1 d .
O3 O 0.6584(2) 0.2846(3) 0.26860(13) 0.0698(5) Uani 1 1 d .
O4 O 0.9470(2) 0.4664(2) 0.24082(14) 0.0650(5) Uani 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 0.0000 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
N2 Cu1 N2 180.0 . 2_655
N2 Cu1 N1 81.26(5) . .
N2 Cu1 N1 98.74(5) 2_655 .
N2 Cu1 N1 98.74(5) . 2_655
N2 Cu1 N1 81.26(5) 2_655 2_655
N1 Cu1 N1 180.0 . 2_655
N2 Cu1 O1 91.70(5) . .
N2 Cu1 O1 88.30(5) 2_655 .
N1 Cu1 O1 88.92(5) . .
N1 Cu1 O1 91.08(5) 2_655 .
N2 Cu1 O1 88.30(5) . 2_655
N2 Cu1 O1 91.70(5) 2_655 2_655
N1 Cu1 O1 91.08(5) . 2_655
N1 Cu1 O1 88.92(5) 2_655 2_655
O1 Cu1 O1 180.0 . 2_655
N1 C1 C2 122.23(14) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C1 C2 C3 119.21(14) . .
C1 C2 H2 120.4 . .
C3 C2 H2 120.4 . .
C2 C3 C4 119.16(15) . .
C2 C3 H3 120.4 . .
C4 C3 H3 120.4 . .
C3 C4 C5 118.45(15) . .
C3 C4 H4 120.8 . .
C5 C4 H4 120.8 . .
N1 C5 C4 122.65(14) . .
N1 C5 C6 113.48(13) . .
C4 C5 C6 123.85(14) . .
N2 C6 C7 107.81(13) . .
N2 C6 C5 117.45(13) . .
C7 C6 C5 134.59(14) . .
N4 C7 C6 104.15(13) . .
N4 C7 H7 127.9 . .
C6 C7 H7 127.9 . .
N4 C8 C9 113.28(12) . .
N4 C8 H8A 108.9 . .
C9 C8 H8A 108.9 . .
N4 C8 H8B 108.9 . .
C9 C8 H8B 108.9 . .
H8A C8 H8B 107.7 . .
N15 C9 C10 123.34(14) . .
N15 C9 C8 116.18(13) . .
C10 C9 C8 120.31(14) . .
C11 C10 C9 118.13(15) . .
C11 C10 H10 120.9 . .
C9 C10 H10 120.9 . .
C10 C11 C12 119.26(15) . .
C10 C11 H11 120.4 . .
C12 C11 H11 120.4 . .
C11 C12 C13 118.73(15) . .
C11 C12 H12 120.6 . .
C13 C12 H12 120.6 . .
N15 C13 C12 122.76(15) . .
N15 C13 C15 115.16(14) . .
C12 C13 C15 122.07(15) . .
C9 N15 C13 117.77(13) . .
N5 C15 C13 112.33(14) . .
N5 C15 H15A 109.1 . .
C13 C15 H15A 109.1 . .
N5 C15 H15B 109.1 . .
C13 C15 H15B 109.1 . .
H15A C15 H15B 107.9 . .
C1 N1 C5 118.25(13) . .
C1 N1 Cu1 127.47(10) . .
C5 N1 Cu1 114.28(10) . .
N3 N2 C6 110.25(12) . .
N3 N2 Cu1 136.27(10) . .
C6 N2 Cu1 113.34(9) . .
N2 N3 N4 105.64(12) . .
N3 N4 C7 112.14(12) . .
N3 N4 C8 118.97(13) . .
C7 N4 C8 128.89(13) . .
N6 N5 C15 115.55(14) . .
N7 N6 N5 170.59(18) . .
O2 Cl1 O3 110.74(12) . .
O2 Cl1 O4 109.96(11) . .
O3 Cl1 O4 109.91(12) . .
O2 Cl1 O1 108.33(9) . .
O3 Cl1 O1 109.62(10) . .
O4 Cl1 O1 108.22(9) . .
Cl1 O1 Cu1 129.40(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.9938(12) .
Cu1 N2 1.9939(12) 2_655
Cu1 N1 2.0380(12) .
Cu1 N1 2.0380(12) 2_655
Cu1 O1 2.4389(12) .
Cu1 O1 2.4389(12) 2_655
C1 N1 1.3431(19) .
C1 C2 1.385(2) .
C1 H1 0.9500 .
C2 C3 1.383(2) .
C2 H2 0.9500 .
C3 C4 1.387(2) .
C3 H3 0.9500 .
C4 C5 1.386(2) .
C4 H4 0.9500 .
C5 N1 1.3508(19) .
C5 C6 1.461(2) .
C6 N2 1.3573(19) .
C6 C7 1.367(2) .
C7 N4 1.349(2) .
C7 H7 0.9500 .
C8 N4 1.4679(19) .
C8 C9 1.512(2) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 N15 1.3370(19) .
C9 C10 1.389(2) .
C10 C11 1.383(2) .
C10 H10 0.9500 .
C11 C12 1.383(2) .
C11 H11 0.9500 .
C12 C13 1.387(2) .
C12 H12 0.9500 .
C13 N15 1.340(2) .
C13 C15 1.509(2) .
C15 N5 1.480(2) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
N2 N3 1.3120(17) .
N3 N4 1.3390(18) .
N5 N6 1.241(2) .
N6 N7 1.130(2) .
Cl1 O2 1.4211(14) .
Cl1 O3 1.4221(16) .
Cl1 O4 1.4273(15) .
Cl1 O1 1.4485(12) .
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
N1 C1 C2 C3 -0.8(3) .
C1 C2 C3 C4 1.6(3) .
C2 C3 C4 C5 -0.5(3) .
C3 C4 C5 N1 -1.5(2) .
C3 C4 C5 C6 176.41(15) .
N1 C5 C6 N2 -2.52(19) .
C4 C5 C6 N2 179.39(14) .
N1 C5 C6 C7 172.35(16) .
C4 C5 C6 C7 -5.7(3) .
N2 C6 C7 N4 0.77(16) .
C5 C6 C7 N4 -174.45(16) .
N4 C8 C9 N15 43.8(2) .
N4 C8 C9 C10 -140.82(15) .
N15 C9 C10 C11 -0.1(2) .
C8 C9 C10 C11 -175.16(15) .
C9 C10 C11 C12 -0.6(2) .
C10 C11 C12 C13 0.6(3) .
C11 C12 C13 N15 0.2(2) .
C11 C12 C13 C15 179.18(16) .
C10 C9 N15 C13 0.9(2) .
C8 C9 N15 C13 176.10(14) .
C12 C13 N15 C9 -0.9(2) .
C15 C13 N15 C9 -179.95(14) .
N15 C13 C15 N5 -78.83(19) .
C12 C13 C15 N5 102.11(18) .
C2 C1 N1 C5 -1.1(2) .
C2 C1 N1 Cu1 178.42(12) .
C4 C5 N1 C1 2.3(2) .
C6 C5 N1 C1 -175.82(13) .
C4 C5 N1 Cu1 -177.29(12) .
C6 C5 N1 Cu1 4.60(16) .
N2 Cu1 N1 C1 176.42(13) .
N2 Cu1 N1 C1 -3.58(13) 2_655
O1 Cu1 N1 C1 84.53(13) .
O1 Cu1 N1 C1 -95.47(13) 2_655
N2 Cu1 N1 C5 -4.04(10) .
N2 Cu1 N1 C5 175.96(10) 2_655
O1 Cu1 N1 C5 -95.93(10) .
O1 Cu1 N1 C5 84.07(10) 2_655
C7 C6 N2 N3 -0.68(17) .
C5 C6 N2 N3 175.49(12) .
C7 C6 N2 Cu1 -177.04(10) .
C5 C6 N2 Cu1 -0.88(16) .
N1 Cu1 N2 N3 -172.50(15) .
N1 Cu1 N2 N3 7.50(15) 2_655
O1 Cu1 N2 N3 -83.85(15) .
O1 Cu1 N2 N3 96.15(15) 2_655
N1 Cu1 N2 C6 2.57(10) .
N1 Cu1 N2 C6 -177.43(10) 2_655
O1 Cu1 N2 C6 91.22(10) .
O1 Cu1 N2 C6 -88.78(10) 2_655
C6 N2 N3 N4 0.27(16) .
Cu1 N2 N3 N4 175.44(11) .
N2 N3 N4 C7 0.24(17) .
N2 N3 N4 C8 -179.53(13) .
C6 C7 N4 N3 -0.64(17) .
C6 C7 N4 C8 179.11(15) .
C9 C8 N4 N3 120.59(15) .
C9 C8 N4 C7 -59.1(2) .
C13 C15 N5 N6 65.5(2) .
O2 Cl1 O1 Cu1 64.45(13) .
O3 Cl1 O1 Cu1 -56.49(14) .
O4 Cl1 O1 Cu1 -176.37(11) .
N2 Cu1 O1 Cl1 32.10(11) .
N2 Cu1 O1 Cl1 -147.90(11) 2_655
N1 Cu1 O1 Cl1 113.32(11) .
N1 Cu1 O1 Cl1 -66.68(11) 2_655
