#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:50:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179939 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/34/7023446.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_7023446
loop_
_publ_author_name
'Liu, Jiang'
'Qin, Ying-Lian'
'Qu, Mei'
'Clérac, Rodolphe'
'Zhang, Xian-Ming'
_publ_section_title
;
 Rung-defected ladder of azido-bridged Cu(II) chains linked by
 [Cu(picolinate)2] units.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11571
_journal_page_last               11575
_journal_paper_doi               10.1039/c3dt51363g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C36 H24 Cu11 N54 O12'
_chemical_formula_weight         2104.03
_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                94.145(7)
_cell_angle_beta                 106.864(6)
_cell_angle_gamma                107.510(5)
_cell_formula_units_Z            1
_cell_length_a                   11.050(3)
_cell_length_b                   12.255(4)
_cell_length_c                   13.652(4)
_cell_measurement_reflns_used    530
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     1661.3(9)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'Dianmond version 3.2'
_computing_publication_material  'pubcif version 1.9.9'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker Apex CCD Diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.1302
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6937
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_T_max  0.8428
_exptl_absorpt_correction_T_min  0.4480
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick 1997'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1033
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.556
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.0793
_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)+(0.0936P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.2280
_reflns_number_gt                2853
_reflns_number_total             5540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51363g.txt
_cod_data_source_block           a
_cod_original_cell_volume        1661.4(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7023446
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 -0.00875(16) 0.31902(13) 0.12800(11) 0.0305(4) Uani 1 1 d .
Cu2 Cu 0.00349(16) 0.57265(13) 0.11357(11) 0.0309(4) Uani 1 1 d .
Cu3 Cu 0.00699(17) 0.82265(13) 0.09688(12) 0.0331(5) Uani 1 1 d .
Cu4 Cu -0.01895(17) 0.06349(13) 0.12702(12) 0.0332(5) Uani 1 1 d .
Cu5 Cu 0.0000 0.5000 0.5000 0.0392(6) Uani 1 2 d S
Cu6 Cu 0.04189(19) 0.80176(16) 0.50155(13) 0.0433(5) Uani 1 1 d .
O1 O -0.0995(11) 0.5875(9) 0.2327(7) 0.056(3) Uani 1 1 d .
O2 O 0.0360(10) 0.6898(9) 0.3904(7) 0.051(3) Uani 1 1 d .
O3 O -0.1467(10) 0.2989(7) 0.2238(7) 0.040(2) Uani 1 1 d .
O4 O -0.0084(9) 0.3932(8) 0.3841(7) 0.043(2) Uani 1 1 d .
O5 O -0.1656(10) 0.0215(8) 0.2152(7) 0.047(3) Uani 1 1 d .
O6 O -0.0366(10) 0.1098(8) 0.3791(7) 0.045(3) Uani 1 1 d .
N1 N -0.1371(12) 0.7835(11) 0.4138(8) 0.044(3) Uani 1 1 d .
N2 N -0.1904(12) 0.4637(10) 0.4255(8) 0.039(3) Uani 1 1 d .
N3 N -0.2340(12) 0.1527(10) 0.4222(8) 0.040(3) Uani 1 1 d .
N4 N -0.1160(11) 0.1565(9) 0.0393(8) 0.028(2) Uani 1 1 d .
N5 N -0.2388(14) 0.1229(10) 0.0080(9) 0.045(3) Uani 1 1 d .
N6 N -0.3535(15) 0.0883(14) -0.0218(14) 0.093(6) Uani 1 1 d .
N7 N 0.1019(11) 0.2240(8) 0.1953(8) 0.033(3) Uani 1 1 d .
N8 N 0.1871(11) 0.2504(9) 0.2795(9) 0.035(3) Uani 1 1 d .
N9 N 0.2680(15) 0.2753(12) 0.3590(10) 0.064(4) Uani 1 1 d .
N10 N -0.1124(11) 0.4105(8) 0.0424(8) 0.029(3) Uani 1 1 d .
N11 N -0.2334(13) 0.3780(10) 0.0119(10) 0.051(4) Uani 1 1 d .
N12 N -0.3469(16) 0.3460(15) -0.0200(16) 0.109(7) Uani 1 1 d .
N13 N 0.1155(12) 0.4806(10) 0.1827(8) 0.039(3) Uani 1 1 d .
N14 N 0.2158(15) 0.5210(10) 0.2599(10) 0.044(3) Uani 1 1 d .
N15 N 0.3118(17) 0.5587(14) 0.3302(13) 0.100(7) Uani 1 1 d .
N16 N -0.1043(11) 0.6617(8) 0.0274(8) 0.031(3) Uani 1 1 d .
N17 N -0.2242(15) 0.6225(10) -0.0125(10) 0.052(4) Uani 1 1 d .
N18 N -0.3379(17) 0.5857(15) -0.0548(15) 0.109(7) Uani 1 1 d .
N19 N 0.1244(12) 0.7363(9) 0.1700(9) 0.039(3) Uani 1 1 d .
N20 N 0.2338(13) 0.7759(10) 0.2326(10) 0.042(3) Uani 1 1 d .
N21 N 0.3393(14) 0.8138(12) 0.2916(13) 0.077(5) Uani 1 1 d .
N22 N -0.1108(12) 0.9083(9) 0.0318(8) 0.037(3) Uani 1 1 d .
N23 N -0.2279(16) 0.8682(11) -0.0214(11) 0.057(4) Uani 1 1 d .
N24 N -0.3389(19) 0.8355(14) -0.0740(17) 0.127(9) Uani 1 1 d .
N25 N 0.1039(11) 0.9761(8) 0.1927(8) 0.030(3) Uani 1 1 d .
N26 N 0.1411(13) 0.9728(10) 0.2856(10) 0.047(3) Uani 1 1 d .
N27 N 0.1764(19) 0.9714(13) 0.3741(11) 0.089(6) Uani 1 1 d .
C1 C -0.0690(17) 0.6609(12) 0.3124(11) 0.043(4) Uani 1 1 d .
C2 C -0.1759(17) 0.7129(13) 0.3185(12) 0.051(4) Uani 1 1 d .
C3 C -0.2968(17) 0.6934(15) 0.2439(12) 0.062(5) Uani 1 1 d .
H3A H -0.3172 0.6482 0.1798 0.074 Uiso 1 1 calc R
C4 C -0.3892(19) 0.7396(18) 0.2622(14) 0.078(6) Uani 1 1 d .
H4A H -0.4724 0.7253 0.2122 0.094 Uiso 1 1 calc R
C5 C -0.3526(18) 0.8090(15) 0.3592(14) 0.064(5) Uani 1 1 d .
H5A H -0.4111 0.8430 0.3745 0.077 Uiso 1 1 calc R
C6 C -0.2277(17) 0.8265(14) 0.4325(12) 0.055(4) Uani 1 1 d .
H6A H -0.2063 0.8703 0.4976 0.066 Uiso 1 1 calc R
C7 C -0.1182(13) 0.3605(11) 0.3093(11) 0.036(3) Uani 1 1 d .
C8 C -0.2307(14) 0.3966(12) 0.3316(10) 0.039(3) Uani 1 1 d .
C9 C -0.3586(16) 0.3659(14) 0.2622(11) 0.052(4) Uani 1 1 d .
H9A H -0.3832 0.3203 0.1975 0.063 Uiso 1 1 calc R
C10 C -0.4478(16) 0.4049(15) 0.2919(12) 0.061(5) Uani 1 1 d .
H10A H -0.5358 0.3840 0.2474 0.073 Uiso 1 1 calc R
C11 C -0.4093(18) 0.4755(15) 0.3880(12) 0.061(5) Uani 1 1 d .
H11A H -0.4695 0.5034 0.4081 0.073 Uiso 1 1 calc R
C12 C -0.2795(16) 0.5024(13) 0.4517(11) 0.048(4) Uani 1 1 d .
H12A H -0.2522 0.5496 0.5160 0.057 Uiso 1 1 calc R
C13 C -0.1487(16) 0.0717(12) 0.3041(12) 0.041(4) Uani 1 1 d .
C14 C -0.2673(15) 0.0900(11) 0.3254(11) 0.038(3) Uani 1 1 d .
C15 C -0.3958(16) 0.0525(12) 0.2571(11) 0.049(4) Uani 1 1 d .
H15A H -0.4172 0.0109 0.1911 0.059 Uiso 1 1 calc R
C16 C -0.4919(17) 0.0787(15) 0.2897(13) 0.060(5) Uani 1 1 d .
H16A H -0.5796 0.0555 0.2444 0.072 Uiso 1 1 calc R
C17 C -0.4607(15) 0.1393(15) 0.3895(13) 0.057(5) Uani 1 1 d .
H17A H -0.5266 0.1549 0.4119 0.068 Uiso 1 1 calc R
C18 C -0.3319(16) 0.1742(14) 0.4520(12) 0.053(4) Uani 1 1 d .
H18A H -0.3096 0.2148 0.5186 0.064 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'
O O 0.0106 0.0060 '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
N13 Cu1 N7 102.9(4) . .
N13 Cu1 N10 78.3(4) . .
N7 Cu1 N10 171.9(4) . .
N13 Cu1 N4 164.5(4) . .
N7 Cu1 N4 78.2(4) . .
N10 Cu1 N4 98.6(4) . .
N13 Cu1 O3 102.4(4) . .
N7 Cu1 O3 99.5(4) . .
N10 Cu1 O3 88.0(4) . .
N4 Cu1 O3 92.6(4) . .
N19 Cu2 N13 102.9(4) . .
N19 Cu2 N10 173.6(4) . .
N13 Cu2 N10 78.5(4) . .
N19 Cu2 N16 78.6(4) . .
N13 Cu2 N16 172.9(4) . .
N10 Cu2 N16 99.3(4) . .
N19 Cu2 O1 88.9(4) . .
N13 Cu2 O1 98.7(4) . .
N10 Cu2 O1 97.2(4) . .
N16 Cu2 O1 88.2(4) . .
N22 Cu3 N16 101.0(4) . .
N22 Cu3 N25 81.2(4) . .
N16 Cu3 N25 167.4(4) . .
N22 Cu3 N19 177.0(5) . .
N16 Cu3 N19 79.7(4) . .
N25 Cu3 N19 97.5(4) . .
N7 Cu4 N22 164.2(5) . 1_545
N7 Cu4 N4 79.7(4) . .
N22 Cu4 N4 98.5(4) 1_545 .
N7 Cu4 N25 98.6(4) . 1_545
N22 Cu4 N25 79.5(4) 1_545 1_545
N4 Cu4 N25 166.8(4) . 1_545
N7 Cu4 O5 103.6(4) . .
N22 Cu4 O5 92.1(4) 1_545 .
N4 Cu4 O5 92.9(4) . .
N25 Cu4 O5 100.2(4) 1_545 .
O4 Cu5 O4 180.000(2) 2_566 .
O4 Cu5 N2 96.1(4) 2_566 .
O4 Cu5 N2 83.9(4) . .
O4 Cu5 N2 83.9(4) 2_566 2_566
O4 Cu5 N2 96.1(4) . 2_566
N2 Cu5 N2 180.0(4) . 2_566
O6 Cu6 N1 96.3(4) 2_566 .
O6 Cu6 O2 170.6(5) 2_566 .
N1 Cu6 O2 83.9(4) . .
O6 Cu6 N3 84.5(4) 2_566 2_566
N1 Cu6 N3 168.6(5) . 2_566
O2 Cu6 N3 97.2(4) . 2_566
C1 O1 Cu2 132.6(10) . .
C1 O2 Cu6 114.5(9) . .
C7 O3 Cu1 124.2(9) . .
C7 O4 Cu5 114.9(8) . .
C13 O5 Cu4 126.2(10) . .
C13 O6 Cu6 114.0(8) . 2_566
C6 N1 C2 116.7(13) . .
C6 N1 Cu6 129.7(10) . .
C2 N1 Cu6 113.5(10) . .
C12 N2 C8 118.0(12) . .
C12 N2 Cu5 129.2(9) . .
C8 N2 Cu5 112.7(9) . .
C18 N3 C14 118.7(13) . .
C18 N3 Cu6 129.4(10) . 2_566
C14 N3 Cu6 111.9(9) . 2_566
N5 N4 Cu4 119.8(9) . .
N5 N4 Cu1 120.2(8) . .
Cu4 N4 Cu1 98.9(4) . .
N6 N5 N4 178.0(15) . .
N8 N7 Cu4 125.6(8) . .
N8 N7 Cu1 127.0(8) . .
Cu4 N7 Cu1 101.5(5) . .
N9 N8 N7 179.7(15) . .
N11 N10 Cu2 123.7(8) . .
N11 N10 Cu1 121.9(9) . .
Cu2 N10 Cu1 100.3(5) . .
N12 N11 N10 177.7(19) . .
N14 N13 Cu1 130.9(9) . .
N14 N13 Cu2 123.9(9) . .
Cu1 N13 Cu2 101.9(5) . .
N15 N14 N13 178.0(17) . .
N17 N16 Cu3 128.0(9) . .
N17 N16 Cu2 122.6(9) . .
Cu3 N16 Cu2 100.2(5) . .
N18 N17 N16 176.9(19) . .
N20 N19 Cu2 131.5(9) . .
N20 N19 Cu3 127.7(9) . .
Cu2 N19 Cu3 100.7(5) . .
N21 N20 N19 179.2(16) . .
N23 N22 Cu3 127.4(9) . .
N23 N22 Cu4 126.6(9) . 1_565
Cu3 N22 Cu4 100.5(5) . 1_565
N24 N23 N22 176.4(17) . .
N26 N25 Cu3 116.3(8) . .
N26 N25 Cu4 123.9(8) . 1_565
Cu3 N25 Cu4 98.9(4) . 1_565
N27 N26 N25 179.0(13) . .
O1 C1 O2 127.0(15) . .
O1 C1 C2 115.8(15) . .
O2 C1 C2 117.0(12) . .
C3 C2 N1 122.3(14) . .
C3 C2 C1 126.8(14) . .
N1 C2 C1 110.8(14) . .
C2 C3 C4 121.0(15) . .
C2 C3 H3A 119.5 . .
C4 C3 H3A 119.5 . .
C3 C4 C5 117.3(17) . .
C3 C4 H4A 121.4 . .
C5 C4 H4A 121.4 . .
C6 C5 C4 119.5(16) . .
C6 C5 H5A 120.3 . .
C4 C5 H5A 120.3 . .
N1 C6 C5 123.1(14) . .
N1 C6 H6A 118.4 . .
C5 C6 H6A 118.4 . .
O3 C7 O4 128.0(13) . .
O3 C7 C8 117.2(12) . .
O4 C7 C8 114.7(12) . .
N2 C8 C9 123.2(13) . .
N2 C8 C7 113.1(13) . .
C9 C8 C7 123.7(12) . .
C10 C9 C8 117.4(14) . .
C10 C9 H9A 121.3 . .
C8 C9 H9A 121.3 . .
C9 C10 C11 120.9(16) . .
C9 C10 H10A 119.5 . .
C11 C10 H10A 119.5 . .
C12 C11 C10 117.6(15) . .
C12 C11 H11A 121.2 . .
C10 C11 H11A 121.2 . .
N2 C12 C11 122.8(13) . .
N2 C12 H12A 118.6 . .
C11 C12 H12A 118.6 . .
O5 C13 O6 125.1(13) . .
O5 C13 C14 118.2(15) . .
O6 C13 C14 116.7(12) . .
N3 C14 C15 121.9(13) . .
N3 C14 C13 112.5(13) . .
C15 C14 C13 125.5(13) . .
C14 C15 C16 117.5(14) . .
C14 C15 H15A 121.3 . .
C16 C15 H15A 121.3 . .
C15 C16 C17 121.5(16) . .
C15 C16 H16A 119.3 . .
C17 C16 H16A 119.3 . .
C18 C17 C16 117.6(14) . .
C18 C17 H17A 121.2 . .
C16 C17 H17A 121.2 . .
N3 C18 C17 122.8(15) . .
N3 C18 H18A 118.6 . .
C17 C18 H18A 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N13 1.979(12) .
Cu1 N7 2.013(10) .
Cu1 N10 2.030(10) .
Cu1 N4 2.058(10) .
Cu1 O3 2.253(9) .
Cu2 N19 1.991(12) .
Cu2 N13 2.003(11) .
Cu2 N10 2.000(10) .
Cu2 N16 2.037(10) .
Cu2 O1 2.265(10) .
Cu3 N22 1.967(11) .
Cu3 N16 1.974(10) .
Cu3 N25 2.003(10) .
Cu3 N19 2.007(10) .
Cu4 N7 1.988(10) .
Cu4 N22 2.014(10) 1_545
Cu4 N4 2.018(10) .
Cu4 N25 2.025(10) 1_545
Cu4 O5 2.249(10) .
Cu5 O4 1.941(9) 2_566
Cu5 O4 1.941(9) .
Cu5 N2 1.947(12) .
Cu5 N2 1.947(12) 2_566
Cu6 O6 1.916(9) 2_566
Cu6 N1 1.928(11) .
Cu6 O2 1.944(9) .
Cu6 N3 1.955(12) 2_566
O1 C1 1.254(15) .
O2 C1 1.260(16) .
O3 C7 1.243(15) .
O4 C7 1.267(14) .
O5 C13 1.256(16) .
O6 C13 1.284(16) .
O6 Cu6 1.916(9) 2_566
N1 C6 1.339(17) .
N1 C2 1.384(17) .
N2 C12 1.335(16) .
N2 C8 1.348(16) .
N3 C18 1.348(17) .
N3 C14 1.369(16) .
N3 Cu6 1.955(12) 2_566
N4 N5 1.222(15) .
N5 N6 1.142(17) .
N7 N8 1.203(14) .
N8 N9 1.138(15) .
N10 N11 1.205(15) .
N11 N12 1.131(17) .
N13 N14 1.225(16) .
N14 N15 1.145(17) .
N16 N17 1.202(16) .
N17 N18 1.146(18) .
N19 N20 1.190(15) .
N20 N21 1.139(16) .
N22 N23 1.210(16) .
N22 Cu4 2.014(10) 1_565
N23 N24 1.154(19) .
N25 N26 1.223(14) .
N25 Cu4 2.025(10) 1_565
N26 N27 1.160(16) .
C1 C2 1.52(2) .
C2 C3 1.36(2) .
C3 C4 1.38(2) .
C3 H3A 0.9300 .
C4 C5 1.40(2) .
C4 H4A 0.9300 .
C5 C6 1.39(2) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 C8 1.539(18) .
C8 C9 1.374(18) .
C9 C10 1.36(2) .
C9 H9A 0.9300 .
C10 C11 1.39(2) .
C10 H10A 0.9300 .
C11 C12 1.37(2) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
C13 C14 1.497(19) .
C14 C15 1.368(19) .
C15 C16 1.374(19) .
C15 H15A 0.9300 .
C16 C17 1.40(2) .
C16 H16A 0.9300 .
C17 C18 1.346(19) .
C17 H17A 0.9300 .
C18 H18A 0.9300 .
