#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:30:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179504 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/01/4340102.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_4340102
loop_
_publ_author_name
'Chen, Jin-Xiang'
'Chen, Ming'
'Ding, Ni-Ni'
'Chen, Wen-Hua'
'Zhang, Wen-Hua'
'Hor, T. S. Andy'
'Young, David J.'
_publ_section_title
;
 Transmetalation of a Dodecahedral Na9 Aggregate-Based Polymer: A Facile
 Route to Water Stable Cu(II) Coordination Networks.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7446
_journal_page_last               7454
_journal_paper_doi               10.1021/ic500789w
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C30 H20 Cu3 N2 O14, 2(H2 O)'
_chemical_formula_sum            'C30 H24 Cu3 N2 O16'
_chemical_formula_weight         859.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-08-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.1480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.2078(3)
_cell_length_b                   18.0634(8)
_cell_length_c                   13.7582(6)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.71
_cell_volume                     1513.65(12)
_computing_cell_refinement       'ApexII (Bruker, 2011)'
_computing_data_collection       'ApexII (Bruker, 2011)'
_computing_data_reduction        'ApexII (Bruker, 2011)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker ApexII'
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22743
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.175
_exptl_absorpt_correction_T_max  0.9181
_exptl_absorpt_correction_T_min  0.4766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0257
_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)+(0.0367P)²+2.5306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3419
_reflns_number_total             3605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500789w_si_002.cif
_cod_data_source_block           cpx4
_cod_depositor_comments
'Adding full bibliography for 4340099--4340103.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4340102
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Cu2 Cu 0.45138(4) 0.436064(13) 0.923363(17) 0.01051(8) Uani 1 1 d .
Cu1 Cu 0.0000 0.5000 1.0000 0.00985(9) Uani 1 2 d S
O1 O 0.3062(2) 0.47502(8) 1.02454(10) 0.0102(3) Uani 1 1 d D
H1O H 0.317(4) 0.4451(12) 1.0676(16) 0.012 Uiso 1 1 d D
O1W O 0.4032(6) 0.5444(2) 0.3755(3) 0.0779(9) Uani 1 1 d D
H1W H 0.472(8) 0.555(3) 0.324(3) 0.094 Uiso 1 1 d D
H2W H 0.498(7) 0.528(3) 0.431(2) 0.094 Uiso 1 1 d D
O2 O 0.2629(2) 0.48666(8) 0.80792(11) 0.0155(3) Uani 1 1 d .
O3 O 0.0227(3) 0.55352(8) 0.87520(11) 0.0167(3) Uani 1 1 d .
O4 O 0.4026(3) 0.60653(9) 0.17879(11) 0.0193(3) Uani 1 1 d .
O5 O 0.0522(3) 0.61526(9) 0.09439(12) 0.0201(3) Uani 1 1 d .
O6 O 0.4277(3) 0.84844(9) 0.49818(12) 0.0207(3) Uani 1 1 d .
O7 O 0.5496(3) 0.85774(11) 0.35583(14) 0.0336(5) Uani 1 1 d .
N1 N -0.0453(3) 0.70118(9) 0.37298(12) 0.0120(3) Uani 1 1 d .
C1 C 0.1144(3) 0.53476(11) 0.80546(15) 0.0123(4) Uani 1 1 d .
C2 C 0.0352(3) 0.57343(11) 0.70769(15) 0.0144(4) Uani 1 1 d .
C3 C 0.1411(4) 0.56351(15) 0.62892(19) 0.0279(6) Uani 1 1 d .
H3 H 0.2673 0.5327 0.6365 0.033 Uiso 1 1 calc R
C4 C 0.0641(4) 0.59820(16) 0.53869(18) 0.0287(6) Uani 1 1 d .
H4 H 0.1381 0.5911 0.4851 0.034 Uiso 1 1 calc R
C5 C -0.1201(3) 0.64319(12) 0.52658(15) 0.0151(4) Uani 1 1 d .
C6 C -0.2239(4) 0.65410(15) 0.60601(18) 0.0264(5) Uani 1 1 d .
H6 H -0.3485 0.6856 0.5988 0.032 Uiso 1 1 calc R
C7 C -0.1474(4) 0.61929(15) 0.69625(17) 0.0257(5) Uani 1 1 d .
H7 H -0.2202 0.6269 0.7501 0.031 Uiso 1 1 calc R
C8 C -0.2172(3) 0.67924(12) 0.42889(15) 0.0160(4) Uani 1 1 d .
H8A H -0.3203 0.6443 0.3884 0.019 Uiso 1 1 calc R
H8B H -0.3014 0.7236 0.4413 0.019 Uiso 1 1 calc R
C9 C -0.0179(3) 0.66160(11) 0.29297(15) 0.0134(4) Uani 1 1 d .
H9 H -0.1191 0.6236 0.2679 0.016 Uiso 1 1 calc R
C10 C 0.1577(3) 0.67655(11) 0.24764(15) 0.0132(4) Uani 1 1 d .
C11 C 0.2985(3) 0.73397(11) 0.28362(15) 0.0138(4) Uani 1 1 d .
H11 H 0.4180 0.7456 0.2524 0.017 Uiso 1 1 calc R
C12 C 0.2654(3) 0.77460(11) 0.36516(15) 0.0132(4) Uani 1 1 d .
C13 C 0.0911(3) 0.75708(11) 0.40950(15) 0.0135(4) Uani 1 1 d .
H13 H 0.0670 0.7842 0.4656 0.016 Uiso 1 1 calc R
C14 C 0.2035(3) 0.62817(11) 0.16376(15) 0.0144(4) Uani 1 1 d .
C15 C 0.4285(3) 0.83336(11) 0.40900(16) 0.0156(4) 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'
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
O1 Cu2 O4 178.38(7) . 3_666
O1 Cu2 O6 94.52(6) . 2_646
O4 Cu2 O6 84.18(7) 3_666 2_646
O1 Cu2 O2 97.06(6) . .
O4 Cu2 O2 83.75(6) 3_666 .
O6 Cu2 O2 154.06(7) 2_646 .
O1 Cu2 O1 83.43(6) . 3_667
O4 Cu2 O1 97.82(6) 3_666 3_667
O6 Cu2 O1 103.90(6) 2_646 3_667
O2 Cu2 O1 100.44(6) . 3_667
O1 Cu1 O1 180.0 . 3_567
O1 Cu1 O3 88.11(6) . 3_567
O1 Cu1 O3 91.89(6) 3_567 3_567
O1 Cu1 O3 91.89(6) . .
O1 Cu1 O3 88.11(6) 3_567 .
O3 Cu1 O3 180.00(8) 3_567 .
Cu1 O1 Cu2 122.90(7) . .
Cu1 O1 Cu2 118.21(6) . 3_667
Cu2 O1 Cu2 96.57(6) . 3_667
Cu1 O1 H1O 103.0(19) . .
Cu2 O1 H1O 107.9(19) . .
Cu2 O1 H1O 107.4(19) 3_667 .
H1W O1W H2W 113(4) . .
C1 O2 Cu2 130.33(13) . .
C1 O3 Cu1 130.14(13) . .
C14 O4 Cu2 124.72(14) . 3_666
C15 O6 Cu2 129.22(14) . 2_656
C9 N1 C13 122.01(17) . .
C9 N1 C8 119.83(17) . .
C13 N1 C8 117.94(17) . .
O3 C1 O2 127.08(19) . .
O3 C1 C2 116.03(17) . .
O2 C1 C2 116.88(18) . .
C3 C2 C7 119.3(2) . .
C3 C2 C1 121.03(19) . .
C7 C2 C1 119.65(19) . .
C2 C3 C4 120.5(2) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C5 C4 C3 120.3(2) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C6 C5 C4 119.1(2) . .
C6 C5 C8 118.30(19) . .
C4 C5 C8 122.52(19) . .
C5 C6 C7 120.6(2) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C2 C7 C6 120.1(2) . .
C2 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
N1 C8 C5 111.91(16) . .
N1 C8 H8A 109.2 . .
C5 C8 H8A 109.2 . .
N1 C8 H8B 109.2 . .
C5 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
N1 C9 C10 119.90(18) . .
N1 C9 H9 120.0 . .
C10 C9 H9 120.0 . .
C9 C10 C11 118.89(18) . .
C9 C10 C14 120.68(18) . .
C11 C10 C14 120.33(18) . .
C10 C11 C12 120.19(19) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C13 C12 C11 119.20(19) . .
C13 C12 C15 120.54(18) . .
C11 C12 C15 120.11(18) . .
N1 C13 C12 119.77(18) . .
N1 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
O5 C14 O4 129.90(19) . .
O5 C14 C10 118.28(19) . .
O4 C14 C10 111.81(18) . .
O7 C15 O6 128.5(2) . .
O7 C15 C12 117.05(19) . .
O6 C15 C12 114.38(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu2 O1 1.9315(14) .
Cu2 O4 1.9701(15) 3_666
Cu2 O6 1.9802(15) 2_646
Cu2 O2 2.0020(15) .
Cu2 O1 2.2228(14) 3_667
Cu1 O1 1.9189(13) .
Cu1 O1 1.9190(13) 3_567
Cu1 O3 1.9990(15) 3_567
Cu1 O3 1.9990(15) .
O1 Cu2 2.2228(14) 3_667
O1 H1O 0.796(17) .
O1W H1W 0.914(19) .
O1W H2W 0.924(19) .
O2 C1 1.263(2) .
O3 C1 1.253(2) .
O4 C14 1.275(3) .
O4 Cu2 1.9700(15) 3_666
O5 C14 1.225(3) .
O6 C15 1.258(3) .
O6 Cu2 1.9801(15) 2_656
O7 C15 1.227(3) .
N1 C9 1.351(3) .
N1 C13 1.351(3) .
N1 C8 1.485(2) .
C1 C2 1.511(3) .
C2 C3 1.383(3) .
C2 C7 1.388(3) .
C3 C4 1.390(3) .
C3 H3 0.9500 .
C4 C5 1.386(3) .
C4 H4 0.9500 .
C5 C6 1.386(3) .
C5 C8 1.510(3) .
C6 C7 1.391(3) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.383(3) .
C9 H9 0.9500 .
C10 C11 1.385(3) .
C10 C14 1.518(3) .
C11 C12 1.389(3) .
C11 H11 0.9500 .
C12 C13 1.377(3) .
C12 C15 1.510(3) .
C13 H13 0.9500 .
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
O1 H1O O7 0.796(17) 1.988(19) 2.726(2) 154(3) 2_646
O1W H1W O2 0.914(19) 2.78(3) 3.606(4) 151(4) 3_666
