#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/54/4505466.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_4505466
loop_
_publ_author_name
'Yang, En-Cui'
'Ding, Bo'
'Liu, Zhong-Yi'
'Yang, You-Li'
'Zhao, Xiao-Jun'
_publ_section_title
;
 Structural Transformation from a Discrete CuII4Cluster to Two Extended
 CuII4+ CuII1Chain-Based Three-Dimensional Frameworks by Changing the
 Spacer Functionality: Synthesis, Crystal Structures, and Magnetic
 Properties
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1185
_journal_paper_doi               10.1021/cg2011666
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C12 H8.13 Cu2.5 N3 O10.06'
_chemical_formula_weight         514.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.9780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.685(2)
_cell_length_b                   7.4317(6)
_cell_length_c                   15.7589(12)
_cell_measurement_reflns_used    3824
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.68
_cell_volume                     2955.3(4)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7182
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2033
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0235
_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)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                2225
_reflns_number_total             2605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2011666_si_004.cif
_cod_data_source_block           n100707a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2955.4(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C12 H8.13 Cu2.50 N3 O10.06'
_cod_database_code               4505466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Cu1 Cu 0.137765(16) 0.24593(6) 0.41975(3) 0.00733(14) Uani 1 1 d .
Cu2 Cu 0.251955(15) 0.13210(6) 0.41502(3) 0.00733(14) Uani 1 1 d .
Cu3 Cu 0.0000 0.48590(8) 0.2500 0.00820(16) Uani 1 2 d S
N1 N 0.13781(12) 0.2499(4) 0.54717(19) 0.0095(6) Uani 1 1 d .
N2 N 0.18430(12) 0.2886(4) 0.61465(19) 0.0096(6) Uani 1 1 d .
N3 N 0.12312(12) 0.2334(4) 0.6746(2) 0.0116(7) Uani 1 1 d .
H3 H 0.1069 0.2182 0.7146 0.014 Uiso 1 1 calc R
O1 O 0.21211(9) 0.1399(3) 0.28636(15) 0.0110(5) Uani 1 1 d .
O2 O 0.13589(10) 0.2565(3) 0.29500(16) 0.0121(6) Uani 1 1 d .
O3 O 0.04237(9) 0.4868(3) 0.17121(15) 0.0112(5) Uani 1 1 d .
O4 O 0.02951(10) 0.1906(4) 0.17541(17) 0.0143(6) Uani 1 1 d .
O5 O 0.06459(9) 0.5006(3) -0.14554(15) 0.0098(5) Uani 1 1 d .
O6 O 0.08174(10) 0.2233(3) -0.18521(16) 0.0108(5) Uani 1 1 d .
O7 O 0.19804(9) -0.0030(3) -0.05065(15) 0.0085(5) Uani 1 1 d .
O8 O 0.20417(10) 0.2795(3) -0.09643(16) 0.0107(5) Uani 1 1 d .
O9 O 0.20477(9) 0.3681(3) 0.46039(15) 0.0085(5) Uani 1 1 d .
H9 H 0.1961 0.4673 0.4327 0.013 Uiso 1 1 d R
O10 O 0.07334(9) 0.0991(3) 0.38718(15) 0.0098(5) Uani 1 1 d .
H10A H 0.0419 0.1366 0.3621 0.015 Uiso 1 1 d R
H10B H 0.0763 0.0070 0.3572 0.015 Uiso 1 1 d R
C1 C 0.17394(15) 0.2776(5) 0.6911(2) 0.0109(8) Uani 1 1 d .
H1 H 0.1989 0.2981 0.7490 0.013 Uiso 1 1 calc R
C2 C 0.10162(15) 0.2164(5) 0.5851(2) 0.0121(8) Uani 1 1 d .
H2 H 0.0658 0.1851 0.5540 0.015 Uiso 1 1 calc R
C3 C 0.14424(14) 0.2278(5) 0.1524(2) 0.0082(7) Uani 1 1 d .
C4 C 0.09347(14) 0.2983(5) 0.1123(2) 0.0089(7) Uani 1 1 d .
C5 C 0.07643(14) 0.3405(5) 0.0220(2) 0.0094(7) Uani 1 1 d .
H5 H 0.0427 0.3950 -0.0043 0.011 Uiso 1 1 calc R
C6 C 0.10815(13) 0.3040(5) -0.0308(2) 0.0070(7) Uani 1 1 d .
C7 C 0.15713(14) 0.2207(4) 0.0070(2) 0.0075(7) Uani 1 1 d .
C8 C 0.17573(14) 0.1867(5) 0.0987(2) 0.0086(7) Uani 1 1 d .
H8 H 0.2099 0.1355 0.1253 0.010 Uiso 1 1 calc R
C9 C 0.16597(14) 0.2048(5) 0.2526(2) 0.0093(7) Uani 1 1 d .
C10 C 0.05281(14) 0.3243(5) 0.1589(2) 0.0112(8) Uani 1 1 d .
C11 C 0.08417(13) 0.3450(5) -0.1289(2) 0.0080(7) Uani 1 1 d .
C12 C 0.18933(13) 0.1669(5) -0.0523(2) 0.0079(7) Uani 1 1 d .
O11 O 0.0000 0.0000 0.5000 0.041(10) Uani 0.13 2 d SP
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
O9 Cu1 O2 91.89(10) . .
O9 Cu1 O10 173.57(10) . .
O2 Cu1 O10 91.47(10) . .
O9 Cu1 N1 87.82(11) . .
O2 Cu1 N1 176.58(11) . .
O10 Cu1 N1 89.15(11) . .
O9 Cu1 O7 78.17(9) . 6_556
O2 Cu1 O7 91.29(9) . 6_556
O10 Cu1 O7 96.28(9) . 6_556
N1 Cu1 O7 91.99(10) . 6_556
O9 Cu2 O7 88.20(10) 7_556 6_556
O9 Cu2 O1 176.00(10) 7_556 .
O7 Cu2 O1 95.78(10) 6_556 .
O9 Cu2 N2 87.99(10) 7_556 7_556
O7 Cu2 N2 167.09(11) 6_556 7_556
O1 Cu2 N2 88.04(11) . 7_556
O9 Cu2 O9 84.01(9) 7_556 .
O7 Cu2 O9 76.73(9) 6_556 .
O1 Cu2 O9 97.22(9) . .
N2 Cu2 O9 115.09(10) 7_556 .
O3 Cu3 O3 179.59(15) . 2
O3 Cu3 O5 90.06(10) . 6_566
O3 Cu3 O5 89.92(10) 2 6_566
O3 Cu3 O5 89.92(10) . 5_565
O3 Cu3 O5 90.06(10) 2 5_565
O5 Cu3 O5 174.15(14) 6_566 5_565
C2 N1 N2 107.4(3) . .
C2 N1 Cu1 133.7(3) . .
N2 N1 Cu1 118.9(2) . .
C1 N2 N1 106.7(3) . .
C1 N2 Cu2 132.7(3) . 7_556
N1 N2 Cu2 120.2(2) . 7_556
C1 N3 C2 106.6(3) . .
C1 N3 H3 126.7 . .
C2 N3 H3 126.7 . .
C9 O1 Cu2 124.9(2) . .
C9 O2 Cu1 135.2(2) . .
C10 O3 Cu3 107.4(2) . .
C11 O5 Cu3 114.4(2) . 5_565
C12 O7 Cu2 128.7(2) . 6
C12 O7 Cu1 129.9(2) . 6
Cu2 O7 Cu1 94.92(9) 6 6
Cu1 O9 Cu2 121.60(11) . 7_556
Cu1 O9 Cu2 94.42(9) . .
Cu2 O9 Cu2 95.99(9) 7_556 .
Cu1 O9 H9 99.8 . .
Cu2 O9 H9 119.8 7_556 .
Cu2 O9 H9 124.3 . .
Cu1 O10 H10A 126.1 . .
Cu1 O10 H10B 111.2 . .
H10A O10 H10B 105.2 . .
N2 C1 N3 109.7(3) . .
N2 C1 H1 125.1 . .
N3 C1 H1 125.1 . .
N1 C2 N3 109.5(3) . .
N1 C2 H2 125.3 . .
N3 C2 H2 125.3 . .
C4 C3 C8 119.4(3) . .
C4 C3 C9 120.3(3) . .
C8 C3 C9 120.3(3) . .
C5 C4 C3 119.8(3) . .
C5 C4 C10 115.1(3) . .
C3 C4 C10 125.0(3) . .
C4 C5 C6 120.7(3) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C7 C6 C5 119.9(3) . .
C7 C6 C11 123.9(3) . .
C5 C6 C11 116.0(3) . .
C8 C7 C6 119.6(3) . .
C8 C7 C12 120.8(3) . .
C6 C7 C12 119.7(3) . .
C7 C8 C3 120.3(3) . .
C7 C8 H8 119.8 . .
C3 C8 H8 119.8 . .
O2 C9 O1 126.4(3) . .
O2 C9 C3 115.3(3) . .
O1 C9 C3 118.3(3) . .
O4 C10 O3 125.3(3) . .
O4 C10 C4 119.2(3) . .
O3 C10 C4 115.2(3) . .
O6 C11 O5 126.3(3) . .
O6 C11 C6 119.3(3) . .
O5 C11 C6 114.2(3) . .
O8 C12 O7 126.2(3) . .
O8 C12 C7 121.3(3) . .
O7 C12 C7 112.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O9 1.920(2) .
Cu1 O2 1.952(2) .
Cu1 O10 1.958(2) .
Cu1 N1 2.008(3) .
Cu1 O7 2.361(2) 6_556
Cu2 O9 1.927(2) 7_556
Cu2 O7 1.947(2) 6_556
Cu2 O1 1.960(2) .
Cu2 N2 1.994(3) 7_556
Cu2 O9 2.400(2) .
Cu3 O3 1.932(2) .
Cu3 O3 1.932(2) 2
Cu3 O5 1.961(2) 6_566
Cu3 O5 1.961(2) 5_565
N1 C2 1.314(5) .
N1 N2 1.376(4) .
N2 C1 1.323(4) .
N2 Cu2 1.994(3) 7_556
N3 C1 1.336(5) .
N3 C2 1.346(5) .
N3 H3 0.8800 .
O1 C9 1.267(4) .
O2 C9 1.260(4) .
O3 C10 1.269(5) .
O4 C10 1.244(5) .
O5 C11 1.261(4) .
O5 Cu3 1.961(2) 5_565
O6 C11 1.254(4) .
O7 C12 1.282(4) .
O7 Cu2 1.947(2) 6
O7 Cu1 2.361(2) 6
O8 C12 1.233(4) .
O9 Cu2 1.927(2) 7_556
O9 H9 0.8499 .
O10 H10A 0.8500 .
O10 H10B 0.8499 .
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 C4 1.397(5) .
C3 C8 1.406(5) .
C3 C9 1.505(5) .
C4 C5 1.381(5) .
C4 C10 1.508(5) .
C5 C6 1.394(5) .
C5 H5 0.9500 .
C6 C7 1.393(5) .
C6 C11 1.500(5) .
C7 C8 1.390(5) .
C7 C12 1.515(4) .
C8 H8 0.9500 .
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_4
O9 Cu1 N1 C2 167.8(3) . .
O2 Cu1 N1 C2 82.6(19) . .
O10 Cu1 N1 C2 -17.9(3) . .
O7 Cu1 N1 C2 -114.2(3) 6_556 .
O9 Cu1 N1 N2 -14.9(2) . .
O2 Cu1 N1 N2 -100.1(19) . .
O10 Cu1 N1 N2 159.5(2) . .
O7 Cu1 N1 N2 63.2(2) 6_556 .
C2 N1 N2 C1 -0.3(4) . .
Cu1 N1 N2 C1 -178.3(2) . .
C2 N1 N2 Cu2 -174.8(2) . 7_556
Cu1 N1 N2 Cu2 7.2(3) . 7_556
O9 Cu2 O1 C9 -129.2(14) 7_556 .
O7 Cu2 O1 C9 55.8(3) 6_556 .
N2 Cu2 O1 C9 -136.6(3) 7_556 .
O9 Cu2 O1 C9 -21.5(3) . .
O9 Cu1 O2 C9 56.6(3) . .
O10 Cu1 O2 C9 -117.9(3) . .
N1 Cu1 O2 C9 141.7(18) . .
O7 Cu1 O2 C9 -21.6(3) 6_556 .
O3 Cu3 O3 C10 177.1(2) 2 .
O5 Cu3 O3 C10 90.0(2) 6_566 .
O5 Cu3 O3 C10 -95.8(2) 5_565 .
O2 Cu1 O9 Cu2 -164.30(14) . 7_556
O10 Cu1 O9 Cu2 -42.8(9) . 7_556
N1 Cu1 O9 Cu2 19.11(15) . 7_556
O7 Cu1 O9 Cu2 -73.38(13) 6_556 7_556
O2 Cu1 O9 Cu2 -64.49(10) . .
O10 Cu1 O9 Cu2 57.0(9) . .
N1 Cu1 O9 Cu2 118.92(10) . .
O7 Cu1 O9 Cu2 26.43(7) 6_556 .
O9 Cu2 O9 Cu1 -122.45(13) 7_556 .
O7 Cu2 O9 Cu1 -32.88(9) 6_556 .
O1 Cu2 O9 Cu1 61.39(10) . .
N2 Cu2 O9 Cu1 152.61(11) 7_556 .
O9 Cu2 O9 Cu2 0.0 7_556 7_556
O7 Cu2 O9 Cu2 89.57(10) 6_556 7_556
O1 Cu2 O9 Cu2 -176.17(10) . 7_556
N2 Cu2 O9 Cu2 -84.94(12) 7_556 7_556
N1 N2 C1 N3 0.2(4) . .
Cu2 N2 C1 N3 173.6(2) 7_556 .
C2 N3 C1 N2 0.1(4) . .
N2 N1 C2 N3 0.4(4) . .
Cu1 N1 C2 N3 178.0(2) . .
C1 N3 C2 N1 -0.3(4) . .
C8 C3 C4 C5 -5.3(5) . .
C9 C3 C4 C5 171.7(3) . .
C8 C3 C4 C10 171.1(3) . .
C9 C3 C4 C10 -11.9(5) . .
C3 C4 C5 C6 3.7(5) . .
C10 C4 C5 C6 -173.0(3) . .
C4 C5 C6 C7 1.3(5) . .
C4 C5 C6 C11 176.3(3) . .
C5 C6 C7 C8 -4.7(5) . .
C11 C6 C7 C8 -179.3(3) . .
C5 C6 C7 C12 174.8(3) . .
C11 C6 C7 C12 0.2(5) . .
C6 C7 C8 C3 3.1(5) . .
C12 C7 C8 C3 -176.3(3) . .
C4 C3 C8 C7 1.8(5) . .
C9 C3 C8 C7 -175.2(3) . .
Cu1 O2 C9 O1 -7.4(6) . .
Cu1 O2 C9 C3 174.0(2) . .
Cu2 O1 C9 O2 -8.2(5) . .
Cu2 O1 C9 C3 170.4(2) . .
C4 C3 C9 O2 -1.5(5) . .
C8 C3 C9 O2 175.5(3) . .
C4 C3 C9 O1 179.8(3) . .
C8 C3 C9 O1 -3.2(5) . .
Cu3 O3 C10 O4 16.3(4) . .
Cu3 O3 C10 C4 -169.8(2) . .
C5 C4 C10 O4 102.5(4) . .
C3 C4 C10 O4 -74.1(5) . .
C5 C4 C10 O3 -71.9(4) . .
C3 C4 C10 O3 111.6(4) . .
Cu3 O5 C11 O6 30.8(4) 5_565 .
Cu3 O5 C11 C6 -143.8(2) 5_565 .
C7 C6 C11 O6 50.0(5) . .
C5 C6 C11 O6 -124.8(3) . .
C7 C6 C11 O5 -135.0(3) . .
C5 C6 C11 O5 50.2(4) . .
Cu2 O7 C12 O8 19.7(5) 6 .
Cu1 O7 C12 O8 -124.6(3) 6 .
Cu2 O7 C12 C7 -160.8(2) 6 .
Cu1 O7 C12 C7 54.8(4) 6 .
C8 C7 C12 O8 -120.5(4) . .
C6 C7 C12 O8 60.0(4) . .
C8 C7 C12 O7 60.0(4) . .
C6 C7 C12 O7 -119.5(3) . .
