#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/84/2018445.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018445
loop_
_publ_author_name
'Zhang, Liangliang'
'Liu, Fuling'
'Yuan, Shuai'
'Wang, Xiaoyang'
'Sun, Di'
_publ_section_title
;
 A one-dimensional coordination polymer based on a di-Schiff base
 supported trinuclear CuII subunit
;
_journal_coeditor_code           BG3148
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m97
_journal_page_last               m99
_journal_paper_doi               10.1107/S0108270112009936
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Cu3 (C14 H10 N2 O4)2 (C H4 O)2]'
_chemical_formula_moiety         'C30 H26 Cu3 N4 O10'
_chemical_formula_sum            'C30 H26 Cu3 N4 O10'
_chemical_formula_weight         793.17
_chemical_name_systematic
;
catena-poly[bis(μ₄-3-{[2-(3-hydroxy-2-
oxidobenzylidene)hydrazinylidene]methyl}benzene-1,2-
diolato)dimethanoltricopper(II)]
;
_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           SHELXL97
_cell_angle_alpha                112.281(3)
_cell_angle_beta                 95.373(4)
_cell_angle_gamma                104.862(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9019(5)
_cell_length_b                   10.2333(7)
_cell_length_c                   10.4441(7)
_cell_measurement_reflns_used    5094
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      54.762
_cell_measurement_theta_min      4.535
_cell_volume                     737.93(9)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9076
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    2.210
_exptl_absorpt_correction_T_max  0.8093
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             401
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3323
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0539P)²+0.1408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                2686
_reflns_number_total             3323
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg3148.cif
_cod_data_source_block           I
_cod_original_cell_volume        737.93(8)
_cod_database_code               2018445
_cod_database_fobs_code          2018445
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Cu Cu1 0.5000 0.5000 0.5000 0.03200(13) Uani d S 1 2
Cu Cu2 0.90273(4) 0.49267(3) 0.62012(3) 0.03312(12) Uani d . 1 1
C C1 0.8328(3) 0.2326(3) 0.3886(3) 0.0345(5) Uani d . 1 1
C C2 0.6733(3) 0.2699(3) 0.3796(3) 0.0321(5) Uani d . 1 1
C C3 0.5243(3) 0.1756(3) 0.2708(3) 0.0339(5) Uani d . 1 1
C C4 0.5307(4) 0.0352(3) 0.1766(3) 0.0412(6) Uani d . 1 1
H H4B 0.4306 -0.0315 0.1063 0.049 Uiso calc R 1 1
C C5 0.6825(4) -0.0021(3) 0.1886(3) 0.0469(7) Uani d . 1 1
H H5A 0.6851 -0.0947 0.1266 0.056 Uiso calc R 1 1
C C6 0.8340(4) 0.0960(3) 0.2922(3) 0.0424(6) Uani d . 1 1
H H6A 0.9377 0.0695 0.2968 0.051 Uiso calc R 1 1
C C7 0.3712(3) 0.2182(3) 0.2412(3) 0.0351(6) Uani d . 1 1
H H7A 0.2764 0.1460 0.1689 0.042 Uiso calc R 1 1
C C8 0.1539(3) 0.3233(3) 0.1124(3) 0.0368(6) Uani d . 1 1
H H8A 0.2303 0.2829 0.0589 0.044 Uiso calc R 1 1
C C9 -0.0040(3) 0.3272(3) 0.0382(3) 0.0374(6) Uani d . 1 1
C C10 -0.1293(3) 0.3860(3) 0.1080(3) 0.0365(6) Uani d . 1 1
C C11 -0.2855(3) 0.3828(3) 0.0252(3) 0.0428(6) Uani d . 1 1
C C12 -0.3109(4) 0.3246(3) -0.1196(3) 0.0498(7) Uani d . 1 1
H H12A -0.4128 0.3236 -0.1728 0.060 Uiso calc R 1 1
C C13 -0.1858(4) 0.2667(3) -0.1886(3) 0.0533(8) Uani d . 1 1
H H13A -0.2045 0.2281 -0.2869 0.064 Uiso calc R 1 1
C C14 -0.0365(4) 0.2669(3) -0.1118(3) 0.0464(7) Uani d . 1 1
H H14A 0.0453 0.2270 -0.1584 0.056 Uiso calc R 1 1
C C15 0.2933(5) 0.1908(4) 0.5662(4) 0.0689(10) Uani d . 1 1
H H15C 0.2137 0.1290 0.4756 0.083 Uiso calc R 1 1
H H15B 0.2452 0.1642 0.6373 0.083 Uiso calc R 1 1
H H15A 0.4085 0.1766 0.5632 0.083 Uiso calc R 1 1
N N1 0.3524(3) 0.3479(2) 0.3057(2) 0.0318(5) Uani d . 1 1
N N2 0.1996(3) 0.3718(2) 0.2492(2) 0.0336(5) Uani d . 1 1
O O1 0.9742(2) 0.33502(19) 0.48878(19) 0.0365(4) Uani d . 1 1
O O2 0.6773(2) 0.40128(19) 0.48112(18) 0.0350(4) Uani d . 1 1
O O3 -0.1134(2) 0.4491(2) 0.24474(19) 0.0400(4) Uani d . 1 1
O O4 -0.4057(3) 0.4399(3) 0.0925(2) 0.0618(6) Uani d D 1 1
H H4A -0.355(4) 0.487(4) 0.181(2) 0.074 Uiso d D 1 1
O O5 0.3112(3) 0.3406(3) 0.5992(2) 0.0536(5) Uani d D 1 1
H H5B 0.214(3) 0.343(4) 0.575(4) 0.064 Uiso d D 1 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Cu1 O2 2_666 . 180.0000(10) ?
O2 Cu1 N1 2_666 . 89.20(7) y
O2 Cu1 N1 . . 90.80(7) y
O2 Cu1 N1 2_666 2_666 90.80(7) ?
O2 Cu1 N1 . 2_666 89.20(7) ?
N1 Cu1 N1 . 2_666 180.0 ?
O2 Cu1 O5 2_666 . 85.99(7) y
O2 Cu1 O5 . . 94.01(7) y
N1 Cu1 O5 . . 86.87(8) y
N1 Cu1 O5 2_666 . 93.13(8) y
O3 Cu2 O1 2_666 . 90.67(8) y
O3 Cu2 O2 2_666 . 170.80(8) y
O1 Cu2 O2 . . 84.41(7) y
O3 Cu2 N2 2_666 2_666 93.42(8) y
O1 Cu2 N2 . 2_666 171.60(8) y
O2 Cu2 N2 . 2_666 90.51(7) y
O3 Cu2 O1 2_666 2_766 95.81(7) y
O1 Cu2 O1 . 2_766 92.16(7) y
O2 Cu2 O1 . 2_766 92.15(7) y
N2 Cu2 O1 2_666 2_766 94.71(7) y
O1 C1 C6 . . 124.6(2) ?
O1 C1 C2 . . 117.0(2) ?
C6 C1 C2 . . 118.4(2) ?
O2 C2 C3 . . 123.5(2) ?
O2 C2 C1 . . 115.6(2) ?
C3 C2 C1 . . 120.8(2) ?
C2 C3 C4 . . 118.5(2) ?
C2 C3 C7 . . 123.3(2) ?
C4 C3 C7 . . 117.9(2) ?
C5 C4 C3 . . 120.2(2) ?
C5 C4 H4B . . 119.9 ?
C3 C4 H4B . . 119.9 ?
C4 C5 C6 . . 120.9(3) ?
C4 C5 H5A . . 119.5 ?
C6 C5 H5A . . 119.5 ?
C1 C6 C5 . . 121.0(3) ?
C1 C6 H6A . . 119.5 ?
C5 C6 H6A . . 119.5 ?
N1 C7 C3 . . 126.2(2) ?
N1 C7 H7A . . 116.9 ?
C3 C7 H7A . . 116.9 ?
N2 C8 C9 . . 125.2(2) ?
N2 C8 H8A . . 117.4 ?
C9 C8 H8A . . 117.4 ?
C10 C9 C14 . . 119.2(2) ?
C10 C9 C8 . . 122.5(2) ?
C14 C9 C8 . . 118.3(2) ?
O3 C10 C9 . . 125.6(2) ?
O3 C10 C11 . . 115.6(2) ?
C9 C10 C11 . . 118.8(2) ?
O4 C11 C12 . . 121.2(3) ?
O4 C11 C10 . . 118.7(3) ?
C12 C11 C10 . . 120.1(3) ?
C11 C12 C13 . . 121.0(3) ?
C11 C12 H12A . . 119.5 ?
C13 C12 H12A . . 119.5 ?
C14 C13 C12 . . 119.9(3) ?
C14 C13 H13A . . 120.0 ?
C12 C13 H13A . . 120.0 ?
C13 C14 C9 . . 121.0(3) ?
C13 C14 H14A . . 119.5 ?
C9 C14 H14A . . 119.5 ?
O5 C15 H15C . . 109.5 ?
O5 C15 H15B . . 109.5 ?
H15C C15 H15B . . 109.5 ?
O5 C15 H15A . . 109.5 ?
H15C C15 H15A . . 109.5 ?
H15B C15 H15A . . 109.5 ?
C7 N1 N2 . . 117.0(2) ?
C7 N1 Cu1 . . 123.56(17) ?
N2 N1 Cu1 . . 118.36(15) ?
C8 N2 N1 . . 118.2(2) ?
C8 N2 Cu2 . 2_666 122.88(18) ?
N1 N2 Cu2 . 2_666 117.85(15) ?
C1 O1 Cu2 . . 110.64(15) ?
C2 O2 Cu1 . . 129.16(15) ?
C2 O2 Cu2 . . 110.84(15) ?
Cu1 O2 Cu2 . . 120.00(8) ?
C10 O3 Cu2 . 2_666 125.08(16) ?
C11 O4 H4A . . 106(3) ?
C15 O5 Cu1 . . 125.9(2) ?
C15 O5 H5B . . 107(3) ?
Cu1 O5 H5B . . 101(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O2 2_666 1.9103(16) ?
Cu1 O2 . 1.9103(16) y
Cu1 N1 . 2.033(2) y
Cu1 N1 2_666 2.033(2) ?
Cu1 O5 . 2.507(2) y
Cu1 Cu2 . 3.3396(3) ?
Cu2 O3 2_666 1.8795(17) y
Cu2 O1 . 1.9332(17) y
Cu2 O2 . 1.9459(16) y
Cu2 N2 2_666 1.946(2) y
Cu2 O1 2_766 2.4894(18) y
C1 O1 . 1.338(3) ?
C1 C6 . 1.381(4) ?
C1 C2 . 1.413(3) ?
C2 O2 . 1.350(3) ?
C2 C3 . 1.394(3) ?
C3 C4 . 1.417(3) ?
C3 C7 . 1.433(3) ?
C4 C5 . 1.358(4) ?
C4 H4B . 0.9300 ?
C5 C6 . 1.389(4) ?
C5 H5A . 0.9300 ?
C6 H6A . 0.9300 ?
C7 N1 . 1.296(3) ?
C7 H7A . 0.9300 ?
C8 N2 . 1.300(3) ?
C8 C9 . 1.423(4) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.408(4) ?
C9 C14 . 1.419(4) ?
C10 O3 . 1.303(3) ?
C10 C11 . 1.425(3) ?
C11 O4 . 1.355(4) ?
C11 C12 . 1.371(4) ?
C12 C13 . 1.400(4) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.362(4) ?
C13 H13A . 0.9300 ?
C14 H14A . 0.9300 ?
C15 O5 . 1.403(4) ?
C15 H15C . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15A . 0.9600 ?
N1 N2 . 1.411(3) ?
N2 Cu2 2_666 1.946(2) ?
O3 Cu2 2_666 1.8795(17) ?
O4 H4A . 0.859(18) ?
O5 H5B . 0.799(17) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O4 H4A O3 . 0.859(18) 2.14(3) 2.638(3) 117(3)
O4 H4A O5 2_566 0.859(18) 2.23(2) 3.029(3) 154(3)
O5 H5B O1 1_455 0.799(17) 1.985(18) 2.779(3) 173(4)
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
C7 N1 N2 C8 -42.6(3)
