#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:27:18 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179664 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/17/4511743.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_4511743
loop_
_publ_author_name
'Li, Shaobin'
'Ma, Huiyuan'
'Pang, Haijun'
'Zhang, Li'
_publ_section_title
;
 Assembly of Six Polyoxometalate-Based Hybrid Compounds from a Simple
 Supramolecule to a Complicated Pseudorotaxane Framework via Tuning the pH
 of the Reaction Systems
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4450
_journal_paper_doi               10.1021/cg5005352
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C21 H22 Cu Mo4 N6 O14'
_chemical_formula_sum            'C21 H22 Cu Mo4 N6 O14'
_chemical_formula_weight         1029.74
_chemical_name_systematic
; 
 ? 
;
_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                67.3010(10)
_cell_angle_beta                 87.7520(10)
_cell_angle_gamma                73.7150(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4391(5)
_cell_length_b                   11.9757(5)
_cell_length_c                   12.3265(6)
_cell_measurement_reflns_used    4317
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.48
_cell_volume                     1490.78(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11498
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             994.0
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0295
_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)+(0.0275P)²+1.5605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                5681
_reflns_number_total             7428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5005352_si_002.cif
_cod_data_source_block           Conpound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511742--4511747.cif.
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4511743
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
Mo1 Mo -0.11564(3) 0.62747(3) 0.01422(3) 0.01688(7) Uani 1 1 d .
Mo2 Mo 0.30114(3) 0.48987(3) 0.09940(3) 0.01673(7) Uani 1 1 d .
Mo3 Mo 0.06332(3) 0.43290(3) 0.24230(3) 0.01775(7) Uani 1 1 d .
Mo4 Mo 0.11389(3) 0.69260(3) -0.13270(3) 0.01778(7) Uani 1 1 d .
Cu1 Cu 0.25983(4) 0.75937(4) 0.19125(4) 0.01689(10) Uani 1 1 d .
O9 O 0.2871(2) 0.6107(2) 0.1492(2) 0.0241(6) Uani 1 1 d .
O11 O 0.0421(3) 0.5583(3) 0.2817(2) 0.0293(6) Uani 1 1 d .
N3 N 0.2427(3) 0.6533(3) 0.3581(2) 0.0214(7) Uani 1 1 d .
O2 O 0.2364(2) 0.3852(2) 0.2319(2) 0.0197(5) Uani 1 1 d .
O4 O 0.2741(2) 0.5904(2) -0.0649(2) 0.0206(5) Uani 1 1 d .
O1 O -0.1048(2) 0.4853(2) 0.1641(2) 0.0180(5) Uani 1 1 d .
O5 O 0.1384(3) 0.7608(3) -0.2767(2) 0.0312(7) Uani 1 1 d .
C1 C 0.3939(4) 0.7988(4) -0.0314(3) 0.0287(9) Uani 1 1 d .
H1 H 0.4331 0.7133 -0.0109 0.034 Uiso 1 1 calc R
C8 C 0.2789(4) 0.5290(3) 0.4139(3) 0.0232(8) Uani 1 1 d .
H8 H 0.3164 0.4731 0.3790 0.028 Uiso 1 1 calc R
N5 N 0.3168(3) 0.8484(3) 0.0358(2) 0.0204(6) Uani 1 1 d .
O7 O 0.4516(2) 0.4140(3) 0.1211(2) 0.0297(6) Uani 1 1 d .
O3 O -0.0610(2) 0.6963(2) -0.1427(2) 0.0178(5) Uani 1 1 d .
O8 O 0.0561(3) 0.3093(3) 0.3681(2) 0.0282(6) Uani 1 1 d .
O6 O -0.2663(2) 0.6452(2) -0.0304(2) 0.0218(5) Uani 1 1 d .
N4 N 0.2544(3) 0.4939(3) 0.5282(3) 0.0228(7) Uani 1 1 d .
N1 N 0.2678(3) 0.8951(3) 0.2450(2) 0.0201(6) Uani 1 1 d .
N2 N 0.3334(3) 0.9706(3) 0.3597(3) 0.0223(7) Uani 1 1 d .
C19 C 0.4401(4) 1.1012(3) 0.3979(3) 0.0246(8) Uani 1 1 d .
C2 C 0.2801(4) 0.9726(3) -0.0248(3) 0.0254(8) Uani 1 1 d .
H2 H 0.2263 1.0300 0.0007 0.030 Uiso 1 1 calc R
C15 C 0.3608(4) 0.8826(3) 0.3128(3) 0.0218(8) Uani 1 1 d .
H15 H 0.4356 0.8211 0.3264 0.026 Uiso 1 1 calc R
O1W O 0.0588(3) 0.8279(3) 0.1423(3) 0.0398(8) Uani 1 1 d .
C12 C 0.2783(4) 0.3667(3) 0.6164(3) 0.0243(8) Uani 1 1 d .
C16 C 0.1752(4) 0.9970(3) 0.2481(3) 0.0314(10) Uani 1 1 d .
H16 H 0.0981 1.0280 0.2084 0.038 Uiso 1 1 calc R
C5 C 0.3616(4) 1.2109(4) -0.1970(3) 0.0257(8) Uani 1 1 d .
H5 H 0.4070 1.1839 -0.1259 0.031 Uiso 1 1 calc R
C20 C 0.5257(4) 1.1186(3) 0.4629(3) 0.0253(8) Uani 1 1 d .
C21 C 0.5570(5) 1.2427(4) 0.4164(4) 0.0410(12) Uani 1 1 d .
H21A H 0.5274 1.2887 0.3349 0.062 Uiso 1 1 calc R
H21B H 0.6440 1.2264 0.4236 0.062 Uiso 1 1 calc R
H21C H 0.5193 1.2916 0.4611 0.062 Uiso 1 1 calc R
C3 C 0.4047(4) 0.8926(4) -0.1322(4) 0.0385(11) Uani 1 1 d .
H3 H 0.4524 0.8841 -0.1930 0.046 Uiso 1 1 calc R
C18 C 0.4173(4) 0.9839(4) 0.4348(3) 0.0223(8) Uani 1 1 d .
C4 C 0.3112(4) 1.1288(3) -0.2175(3) 0.0257(9) Uani 1 1 d .
C6 C 0.2428(4) 1.1618(4) -0.3213(3) 0.0327(10) Uani 1 1 d .
C14 C 0.4062(4) 0.4206(4) 0.7447(4) 0.0374(10) Uani 1 1 d .
H14A H 0.4350 0.4703 0.6733 0.056 Uiso 1 1 calc R
H14B H 0.4737 0.3712 0.8030 0.056 Uiso 1 1 calc R
H14C H 0.3474 0.4755 0.7734 0.056 Uiso 1 1 calc R
N6 N 0.3313(3) 1.0037(3) -0.1279(3) 0.0270(7) Uani 1 1 d .
C9 C 0.1901(4) 0.6981(4) 0.4418(3) 0.0275(9) Uani 1 1 d .
H9 H 0.1549 0.7829 0.4279 0.033 Uiso 1 1 calc R
C13 C 0.3469(4) 0.3335(4) 0.7204(3) 0.0242(8) Uani 1 1 d .
C10 C 0.1971(4) 0.6012(4) 0.5463(3) 0.0301(9) Uani 1 1 d .
H10 H 0.1687 0.6063 0.6165 0.036 Uiso 1 1 calc R
O12 O 0.0771(2) 0.5429(2) 0.04726(19) 0.0169(5) Uani 1 1 d .
O13 O -0.1269(2) 0.7469(2) 0.0586(2) 0.0251(6) Uani 1 1 d .
O14 O 0.0904(3) 0.8100(2) -0.0815(2) 0.0273(6) Uani 1 1 d .
C17 C 0.2154(4) 1.0442(4) 0.3186(4) 0.0319(10) Uani 1 1 d .
H17 H 0.1719 1.1128 0.3358 0.038 Uiso 1 1 calc R
C11 C 0.2267(4) 0.2851(4) 0.5952(3) 0.0325(10) Uani 1 1 d .
H11 H 0.1805 0.3123 0.5246 0.039 Uiso 1 1 calc R
C7 C 0.1815(5) 1.0753(4) -0.3432(4) 0.0518(14) Uani 1 1 d .
H7A H 0.2416 1.0108 -0.3595 0.078 Uiso 1 1 calc R
H7B H 0.1220 1.1233 -0.4095 0.078 Uiso 1 1 calc R
H7C H 0.1417 1.0368 -0.2746 0.078 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'
Mo Mo -1.6832 0.6857 '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
O13 Mo1 O6 104.93(12) . .
O13 Mo1 O3 100.69(11) . .
O6 Mo1 O3 96.98(11) . .
O13 Mo1 O1 101.87(11) . .
O6 Mo1 O1 96.29(11) . .
O3 Mo1 O1 149.83(10) . .
O13 Mo1 O12 98.50(11) . .
O6 Mo1 O12 156.56(10) . .
O3 Mo1 O12 78.66(9) . .
O1 Mo1 O12 78.41(9) . .
O13 Mo1 O12 173.89(11) . 2_565
O6 Mo1 O12 81.03(10) . 2_565
O3 Mo1 O12 77.00(9) . 2_565
O1 Mo1 O12 78.48(9) . 2_565
O12 Mo1 O12 75.54(9) . 2_565
O13 Mo1 Mo3 90.68(9) . .
O6 Mo1 Mo3 132.84(8) . .
O3 Mo1 Mo3 123.89(7) . .
O1 Mo1 Mo3 36.57(7) . .
O12 Mo1 Mo3 45.26(6) . .
O12 Mo1 Mo3 86.05(6) 2_565 .
O7 Mo2 O9 104.05(13) . .
O7 Mo2 O4 104.75(12) . .
O9 Mo2 O4 98.22(11) . .
O7 Mo2 O2 102.87(12) . .
O9 Mo2 O2 96.03(11) . .
O4 Mo2 O2 144.64(11) . .
O7 Mo2 O6 90.82(11) . 2_565
O9 Mo2 O6 165.08(11) . 2_565
O4 Mo2 O6 78.85(10) . 2_565
O2 Mo2 O6 79.12(10) . 2_565
O7 Mo2 O12 160.64(11) . .
O9 Mo2 O12 95.26(10) . .
O4 Mo2 O12 73.46(9) . .
O2 Mo2 O12 73.14(9) . .
O6 Mo2 O12 69.85(8) 2_565 .
O8 Mo3 O11 105.60(13) . .
O8 Mo3 O2 98.35(12) . .
O11 Mo3 O2 101.87(12) . .
O8 Mo3 O1 101.32(12) . .
O11 Mo3 O1 96.42(12) . .
O2 Mo3 O1 148.36(10) . .
O8 Mo3 O12 158.81(11) . .
O11 Mo3 O12 95.51(11) . .
O2 Mo3 O12 78.74(9) . .
O1 Mo3 O12 73.96(9) . .
O8 Mo3 O3 86.91(10) . 2_565
O11 Mo3 O3 164.45(11) . 2_565
O2 Mo3 O3 85.01(9) . 2_565
O1 Mo3 O3 71.64(9) . 2_565
O12 Mo3 O3 71.96(8) . 2_565
O8 Mo3 Mo1 136.69(9) . .
O11 Mo3 Mo1 85.74(9) . .
O2 Mo3 Mo1 120.46(7) . .
O1 Mo3 Mo1 35.38(7) . .
O12 Mo3 Mo1 41.75(6) . .
O3 Mo3 Mo1 78.77(6) 2_565 .
O5 Mo4 O14 104.83(13) . .
O5 Mo4 O4 101.84(13) . .
O14 Mo4 O4 102.08(12) . .
O5 Mo4 O3 101.80(12) . .
O14 Mo4 O3 96.33(11) . .
O4 Mo4 O3 145.03(10) . .
O5 Mo4 O1 89.02(11) . 2_565
O14 Mo4 O1 163.40(11) . 2_565
O4 Mo4 O1 83.55(9) . 2_565
O3 Mo4 O1 71.48(9) . 2_565
O5 Mo4 O12 160.54(11) . .
O14 Mo4 O12 94.34(11) . .
O4 Mo4 O12 76.90(9) . .
O3 Mo4 O12 72.25(9) . .
O1 Mo4 O12 71.53(8) 2_565 .
O9 Cu1 N5 88.07(11) . .
O9 Cu1 N3 90.11(11) . .
N5 Cu1 N3 167.11(13) . .
O9 Cu1 N1 168.48(12) . .
N5 Cu1 N1 91.04(12) . .
N3 Cu1 N1 88.20(12) . .
O9 Cu1 O1W 94.63(11) . .
N5 Cu1 O1W 99.11(13) . .
N3 Cu1 O1W 93.75(13) . .
N1 Cu1 O1W 96.84(12) . .
Mo2 O9 Cu1 174.14(16) . .
C8 N3 C9 105.1(3) . .
C8 N3 Cu1 129.3(3) . .
C9 N3 Cu1 125.6(2) . .
Mo2 O2 Mo3 117.82(12) . .
Mo2 O4 Mo4 120.19(13) . .
Mo1 O1 Mo3 108.05(11) . .
Mo1 O1 Mo4 110.61(10) . 2_565
Mo3 O1 Mo4 103.58(10) . 2_565
C3 C1 N5 109.4(3) . .
N3 C8 N4 111.1(3) . .
C2 N5 C1 106.6(3) . .
C2 N5 Cu1 124.5(3) . .
C1 N5 Cu1 128.9(2) . .
Mo1 O3 Mo4 110.41(11) . .
Mo1 O3 Mo3 109.98(10) . 2_565
Mo4 O3 Mo3 104.40(10) . 2_565
Mo1 O6 Mo2 119.18(12) . 2_565
C8 N4 C10 107.7(3) . .
C8 N4 C12 127.3(3) . .
C10 N4 C12 125.0(3) . .
C15 N1 C16 106.2(3) . .
C15 N1 Cu1 122.2(3) . .
C16 N1 Cu1 129.6(3) . .
C15 N2 C17 107.2(3) . .
C15 N2 C18 124.4(3) . .
C17 N2 C18 128.4(3) . .
C20 C19 C18 120.0(3) . .
N5 C2 N6 110.6(3) . .
N1 C15 N2 111.1(3) . .
C11 C12 C13 122.8(3) . .
C11 C12 N4 118.0(3) . .
C13 C12 N4 119.1(3) . .
C17 C16 N1 108.8(3) . .
C4 C5 C13 122.0(4) . 1_564
C18 C20 C19 117.1(3) 2_676 .
C18 C20 C21 123.5(4) 2_676 .
C19 C20 C21 119.3(3) . .
C1 C3 N6 106.7(4) . .
C20 C18 C19 122.9(3) 2_676 .
C20 C18 N2 120.2(3) 2_676 .
C19 C18 N2 116.9(3) . .
C5 C4 C6 122.4(3) . .
C5 C4 N6 118.5(3) . .
C6 C4 N6 119.1(4) . .
C4 C6 C11 116.1(4) . 1_564
C4 C6 C7 123.3(4) . .
C11 C6 C7 120.5(4) 1_564 .
C2 N6 C3 106.8(3) . .
C2 N6 C4 126.3(3) . .
C3 N6 C4 126.8(3) . .
C10 C9 N3 110.2(3) . .
C12 C13 C5 115.7(3) . 1_546
C12 C13 C14 123.8(3) . .
C5 C13 C14 120.5(4) 1_546 .
C9 C10 N4 106.0(3) . .
Mo1 O12 Mo3 93.00(9) . .
Mo1 O12 Mo4 91.82(8) . .
Mo3 O12 Mo4 163.10(11) . .
Mo1 O12 Mo1 104.46(9) . 2_565
Mo3 O12 Mo1 97.89(8) . 2_565
Mo4 O12 Mo1 96.57(8) . 2_565
Mo1 O12 Mo2 165.55(11) . .
Mo3 O12 Mo2 86.18(8) . .
Mo4 O12 Mo2 85.13(7) . .
Mo1 O12 Mo2 89.94(8) 2_565 .
C16 C17 N2 106.6(3) . .
C12 C11 C6 121.0(4) . 1_546
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O13 1.690(2) .
Mo1 O6 1.760(3) .
Mo1 O3 1.943(2) .
Mo1 O1 1.949(2) .
Mo1 O12 2.134(2) .
Mo1 O12 2.365(2) 2_565
Mo1 Mo3 3.2009(4) .
Mo2 O7 1.682(3) .
Mo2 O9 1.745(2) .
Mo2 O4 1.899(2) .
Mo2 O2 1.906(2) .
Mo2 O6 2.225(2) 2_565
Mo2 O12 2.507(2) .
Mo3 O8 1.700(3) .
Mo3 O11 1.702(3) .
Mo3 O2 1.914(2) .
Mo3 O1 2.006(2) .
Mo3 O12 2.277(2) .
Mo3 O3 2.322(2) 2_565
Mo4 O5 1.694(3) .
Mo4 O14 1.705(2) .
Mo4 O4 1.905(3) .
Mo4 O3 1.996(2) .
Mo4 O1 2.337(2) 2_565
Mo4 O12 2.365(2) .
Cu1 O9 1.981(2) .
Cu1 N5 1.987(3) .
Cu1 N3 1.994(3) .
Cu1 N1 2.002(3) .
Cu1 O1W 2.235(3) .
N3 C8 1.322(4) .
N3 C9 1.383(4) .
O1 Mo4 2.337(2) 2_565
C1 C3 1.345(5) .
C1 N5 1.358(5) .
C8 N4 1.348(4) .
N5 C2 1.328(4) .
O3 Mo3 2.322(2) 2_565
O6 Mo2 2.225(2) 2_565
N4 C10 1.366(5) .
N4 C12 1.445(4) .
N1 C15 1.318(5) .
N1 C16 1.387(5) .
N2 C15 1.347(4) .
N2 C17 1.377(5) .
N2 C18 1.439(4) .
C19 C20 1.395(5) .
C19 C18 1.397(5) .
C2 N6 1.340(5) .
C12 C11 1.381(5) .
C12 C13 1.388(5) .
C16 C17 1.357(5) .
C5 C4 1.373(5) .
C5 C13 1.393(5) 1_564
C20 C18 1.394(5) 2_676
C20 C21 1.513(5) .
C3 N6 1.380(5) .
C18 C20 1.394(5) 2_676
C4 C6 1.386(6) .
C4 N6 1.437(4) .
C6 C11 1.401(5) 1_564
C6 C7 1.508(6) .
C14 C13 1.514(5) .
C9 C10 1.347(5) .
C13 C5 1.393(5) 1_546
O12 Mo1 2.365(2) 2_565
C11 C6 1.401(5) 1_546
