#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:23:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179058 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/20/4302070.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_4302070
loop_
_publ_author_name
'Christer B. Aakeröy'
'Benjamin M. T. Scott'
'Michelle M. Smith'
'Joaquin F. Urbina'
'John Desper'
_publ_section_title
;
Establishing Amide...Amide Reliability and Synthon Transferability in
the Supramolecular Assembly of Metal-Containing One-Dimensional
Architectures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4052
_journal_page_last               4061
_journal_paper_doi               10.1021/ic801992t
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
;
(C2 H3 O2)4 Cu2 (C11 H11 N3 O1)2
;
_chemical_formula_sum            'C30 H34 Cu2 N6 O10'
_chemical_formula_weight         765.71
_chemical_name_systematic
;
mu(OAc)4 Cu2 {3-[(pyrazol-1-yl)methyl]benzamide}2
;
_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                110.1640(10)
_cell_angle_beta                 109.1250(10)
_cell_angle_gamma                90.5040(10)
_cell_formula_units_Z            1
_cell_length_a                   8.0173(4)
_cell_length_b                   10.1615(5)
_cell_length_c                   11.4846(6)
_cell_measurement_reflns_used    5195
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.35
_cell_volume                     821.95(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9572
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0304
_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)+(0.0400P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                4413
_reflns_number_total             4714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801992t_si_002_11.cif
_cod_data_source_block           6b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4302070
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
Cu1 Cu 0.53173(2) 0.140542(17) 0.053893(16) 0.01027(6) Uani 1 1 d . . .
N11 N 0.47706(17) 0.47138(13) 0.14511(12) 0.0142(2) Uani 1 1 d . . .
N12 N 0.58862(17) 0.37200(13) 0.14008(12) 0.0126(2) Uani 1 1 d . . .
C13 C 0.7472(2) 0.44072(16) 0.16576(15) 0.0158(3) Uani 1 1 d . . .
H13 H 0.8525 0.3978 0.1688 0.019 Uiso 1 1 calc R . .
C14 C 0.7374(2) 0.58430(16) 0.18763(15) 0.0187(3) Uani 1 1 d . . .
H14 H 0.8311 0.6556 0.2081 0.022 Uiso 1 1 calc R . .
C15 C 0.5628(2) 0.59928(16) 0.17301(15) 0.0183(3) Uani 1 1 d . . .
H15 H 0.5115 0.6844 0.1811 0.022 Uiso 1 1 calc R . .
C21 C 0.1751(2) 0.66912(15) 0.42583(14) 0.0141(3) Uani 1 1 d . . .
C22 C 0.2040(2) 0.61998(15) 0.30545(14) 0.0143(3) Uani 1 1 d . . .
H22 H 0.1830 0.6764 0.2525 0.017 Uiso 1 1 calc R . .
C23 C 0.2630(2) 0.49009(15) 0.26181(15) 0.0157(3) Uani 1 1 d . . .
C24 C 0.2931(2) 0.40718(17) 0.34042(17) 0.0204(3) Uani 1 1 d . . .
H24 H 0.3331 0.3179 0.3118 0.024 Uiso 1 1 calc R . .
C25 C 0.2643(2) 0.45550(18) 0.46001(17) 0.0223(3) Uani 1 1 d . . .
H25 H 0.2850 0.3990 0.5129 0.027 Uiso 1 1 calc R . .
C26 C 0.2054(2) 0.58586(17) 0.50318(15) 0.0187(3) Uani 1 1 d . . .
H26 H 0.1859 0.6181 0.5851 0.022 Uiso 1 1 calc R . .
C27 C 0.1045(2) 0.80811(15) 0.46113(14) 0.0141(3) Uani 1 1 d . . .
N27 N 0.0862(2) 0.86352(16) 0.57907(13) 0.0199(3) Uani 1 1 d . . .
H27A H 0.054(3) 0.938(2) 0.597(2) 0.024 Uiso 1 1 d . . .
H27B H 0.121(3) 0.829(2) 0.635(2) 0.024 Uiso 1 1 d . . .
O27 O 0.06245(17) 0.86810(12) 0.38036(11) 0.0205(2) Uani 1 1 d . . .
C28 C 0.2912(2) 0.43966(16) 0.13067(15) 0.0178(3) Uani 1 1 d . . .
H28A H 0.2540 0.3361 0.0867 0.021 Uiso 1 1 calc R . .
H28B H 0.2148 0.4853 0.0730 0.021 Uiso 1 1 calc R . .
C31 C 0.83394(19) -0.00228(15) 0.09545(13) 0.0124(3) Uani 1 1 d . . .
O31 O 0.78670(14) 0.11975(11) 0.12414(11) 0.0159(2) Uani 1 1 d . . .
O32 O 0.72933(15) -0.11662(12) 0.02843(11) 0.0184(2) Uani 1 1 d . . .
C32 C 1.0297(2) -0.01342(17) 0.14620(15) 0.0171(3) Uani 1 1 d . . .
H32A H 1.0567 -0.0434 0.2221 0.021 Uiso 1 1 calc R . .
H32B H 1.0989 0.0790 0.1738 0.021 Uiso 1 1 calc R . .
H32C H 1.0611 -0.0831 0.0758 0.021 Uiso 1 1 calc R . .
C41 C 0.47371(19) -0.00337(15) 0.21341(14) 0.0125(3) Uani 1 1 d . . .
O41 O 0.50553(15) 0.11725(11) 0.21052(10) 0.0165(2) Uani 1 1 d . . .
O42 O 0.44608(16) -0.11931(11) 0.11790(10) 0.0170(2) Uani 1 1 d . . .
C42 C 0.4719(2) -0.00884(17) 0.34268(14) 0.0174(3) Uani 1 1 d . . .
H42A H 0.5795 -0.0448 0.3841 0.021 Uiso 1 1 calc R . .
H42B H 0.3663 -0.0717 0.3258 0.021 Uiso 1 1 calc R . .
H42C H 0.4688 0.0865 0.4021 0.021 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
_geom_angle_publ_flag
O32 Cu1 O41 89.50(5) 2_655 . ?
O32 Cu1 O42 89.88(5) 2_655 2_655 ?
O41 Cu1 O42 167.74(4) . 2_655 ?
O32 Cu1 O31 167.67(4) 2_655 . ?
O41 Cu1 O31 88.19(5) . . ?
O42 Cu1 O31 89.82(5) 2_655 . ?
O32 Cu1 N12 100.00(5) 2_655 . ?
O41 Cu1 N12 95.92(4) . . ?
O42 Cu1 N12 96.25(4) 2_655 . ?
O31 Cu1 N12 92.28(4) . . ?
O32 Cu1 Cu1 80.82(3) 2_655 2_655 ?
O41 Cu1 Cu1 85.24(3) . 2_655 ?
O42 Cu1 Cu1 82.57(3) 2_655 2_655 ?
O31 Cu1 Cu1 86.92(3) . 2_655 ?
N12 Cu1 Cu1 178.58(3) . 2_655 ?
C15 N11 N12 111.32(13) . . ?
C15 N11 C28 126.49(13) . . ?
N12 N11 C28 122.05(12) . . ?
C13 N12 N11 105.21(12) . . ?
C13 N12 Cu1 121.98(10) . . ?
N11 N12 Cu1 130.57(10) . . ?
N12 C13 C14 111.03(14) . . ?
N12 C13 H13 124.5 . . ?
C14 C13 H13 124.5 . . ?
C15 C14 C13 104.79(14) . . ?
C15 C14 H14 127.6 . . ?
C13 C14 H14 127.6 . . ?
N11 C15 C14 107.65(13) . . ?
N11 C15 H15 126.2 . . ?
C14 C15 H15 126.2 . . ?
C26 C21 C22 119.35(13) . . ?
C26 C21 C27 123.73(13) . . ?
C22 C21 C27 116.87(13) . . ?
C23 C22 C21 121.16(14) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 119.01(14) . . ?
C22 C23 C28 119.77(14) . . ?
C24 C23 C28 121.21(13) . . ?
C25 C24 C23 120.02(14) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.64(15) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 119.82(14) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
O27 C27 N27 121.41(14) . . ?
O27 C27 C21 119.75(13) . . ?
N27 C27 C21 118.83(13) . . ?
C27 N27 H27A 117.5(16) . . ?
C27 N27 H27B 122.3(16) . . ?
H27A N27 H27B 120(2) . . ?
N11 C28 C23 112.57(12) . . ?
N11 C28 H28A 109.1 . . ?
C23 C28 H28A 109.1 . . ?
N11 C28 H28B 109.1 . . ?
C23 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
O32 C31 O31 125.06(14) . . ?
O32 C31 C32 116.92(13) . . ?
O31 C31 C32 118.02(13) . . ?
C31 O31 Cu1 119.57(10) . . ?
C31 O32 Cu1 127.56(10) . 2_655 ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O42 C41 O41 125.32(13) . . ?
O42 C41 C42 117.44(13) . . ?
O41 C41 C42 117.23(13) . . ?
C41 O41 Cu1 121.93(9) . . ?
C41 O42 Cu1 124.73(9) . 2_655 ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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 O32 1.9671(11) 2_655 ?
Cu1 O41 1.9688(10) . ?
Cu1 O42 1.9768(10) 2_655 ?
Cu1 O31 1.9795(11) . ?
Cu1 N12 2.1908(12) . ?
Cu1 Cu1 2.6596(3) 2_655 ?
N11 C15 1.3481(19) . ?
N11 N12 1.3538(16) . ?
N11 C28 1.464(2) . ?
N12 C13 1.3369(19) . ?
C13 C14 1.400(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(2) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C21 C26 1.394(2) . ?
C21 C22 1.397(2) . ?
C21 C27 1.500(2) . ?
C22 C23 1.388(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.403(2) . ?
C23 C28 1.508(2) . ?
C24 C25 1.388(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 O27 1.2387(18) . ?
C27 N27 1.3337(19) . ?
N27 H27A 0.78(2) . ?
N27 H27B 0.81(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C31 O32 1.2606(18) . ?
C31 O31 1.2642(17) . ?
C31 C32 1.505(2) . ?
O32 Cu1 1.9671(11) 2_655 ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O42 1.2592(17) . ?
C41 O41 1.2636(17) . ?
C41 C42 1.5093(19) . ?
O42 Cu1 1.9768(10) 2_655 ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N27 H27A O27 0.78(2) 2.16(2) 2.9359(18) 172(2) 2_576
N27 H27B O31 0.81(2) 2.47(2) 3.1634(18) 144(2) 2_666
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
C15 N11 N12 C13 0.09(16) . . . . ?
C28 N11 N12 C13 -175.91(13) . . . . ?
C15 N11 N12 Cu1 -162.71(10) . . . . ?
C28 N11 N12 Cu1 21.29(19) . . . . ?
O32 Cu1 N12 C13 -155.78(11) 2_655 . . . ?
O41 Cu1 N12 C13 113.68(11) . . . . ?
O42 Cu1 N12 C13 -64.80(12) 2_655 . . . ?
O31 Cu1 N12 C13 25.27(11) . . . . ?
O32 Cu1 N12 N11 4.56(13) 2_655 . . . ?
O41 Cu1 N12 N11 -85.98(12) . . . . ?
O42 Cu1 N12 N11 95.54(12) 2_655 . . . ?
O31 Cu1 N12 N11 -174.39(12) . . . . ?
N11 N12 C13 C14 0.16(16) . . . . ?
Cu1 N12 C13 C14 164.81(10) . . . . ?
N12 C13 C14 C15 -0.34(17) . . . . ?
N12 N11 C15 C14 -0.30(17) . . . . ?
C28 N11 C15 C14 175.48(14) . . . . ?
C13 C14 C15 N11 0.38(17) . . . . ?
C26 C21 C22 C23 -0.3(2) . . . . ?
C27 C21 C22 C23 -177.63(14) . . . . ?
C21 C22 C23 C24 0.3(2) . . . . ?
C21 C22 C23 C28 179.44(14) . . . . ?
C22 C23 C24 C25 -0.2(2) . . . . ?
C28 C23 C24 C25 -179.34(15) . . . . ?
C23 C24 C25 C26 0.1(3) . . . . ?
C24 C25 C26 C21 -0.1(3) . . . . ?
C22 C21 C26 C25 0.2(2) . . . . ?
C27 C21 C26 C25 177.36(15) . . . . ?
C26 C21 C27 O27 -171.96(15) . . . . ?
C22 C21 C27 O27 5.3(2) . . . . ?
C26 C21 C27 N27 7.2(2) . . . . ?
C22 C21 C27 N27 -175.57(14) . . . . ?
C15 N11 C28 C23 -74.25(19) . . . . ?
N12 N11 C28 C23 101.12(15) . . . . ?
C22 C23 C28 N11 96.15(17) . . . . ?
C24 C23 C28 N11 -84.69(18) . . . . ?
O32 C31 O31 Cu1 -3.27(19) . . . . ?
C32 C31 O31 Cu1 177.60(9) . . . . ?
O32 Cu1 O31 C31 8.7(3) 2_655 . . . ?
O41 Cu1 O31 C31 87.97(11) . . . . ?
O42 Cu1 O31 C31 -79.93(11) 2_655 . . . ?
N12 Cu1 O31 C31 -176.18(10) . . . . ?
Cu1 Cu1 O31 C31 2.64(10) 2_655 . . . ?
O31 C31 O32 Cu1 1.6(2) . . . 2_655 ?
C32 C31 O32 Cu1 -179.25(9) . . . 2_655 ?
O42 C41 O41 Cu1 -4.0(2) . . . . ?
C42 C41 O41 Cu1 174.91(10) . . . . ?
O32 Cu1 O41 C41 81.47(12) 2_655 . . . ?
O42 Cu1 O41 C41 -5.6(3) 2_655 . . . ?
O31 Cu1 O41 C41 -86.42(12) . . . . ?
N12 Cu1 O41 C41 -178.53(11) . . . . ?
Cu1 Cu1 O41 C41 0.64(11) 2_655 . . . ?
O41 C41 O42 Cu1 6.0(2) . . . 2_655 ?
C42 C41 O42 Cu1 -172.87(10) . . . 2_655 ?
