#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:17:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179962 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/56/7025605.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_7025605
loop_
_publ_author_name
'Zhang, Chun-Jing'
'Pang, Hai-Jun'
'Tang, Qun'
'Wang, Hui-Yuan'
'Chen, Ya-Guang'
_publ_section_title
;
 Tailoring microstructures of isopolymolybdates: regular tuning of the
 ligand spacer length and metal coordination preferences.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7993
_journal_page_last               7999
_journal_paper_doi               10.1039/c002037k
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C14 H26 Cu Mo4 N12 O16'
_chemical_formula_weight         1065.78
_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                71.1380(12)
_cell_angle_beta                 77.1160(12)
_cell_angle_gamma                85.8450(14)
_cell_formula_units_Z            2
_cell_length_a                   11.6710(12)
_cell_length_b                   11.7000(12)
_cell_length_c                   11.9010(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     1499.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      293(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8055
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1038.0
_exptl_crystal_size_max          0.1121
_exptl_crystal_size_mid          0.1116
_exptl_crystal_size_min          0.1111
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0325
_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)+(0.0357P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                4298
_reflns_number_total             5737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002037k.txt
_cod_data_source_block           compound4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7025605
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 0.46078(3) 0.50438(3) 0.36226(3) 0.02701(10) Uani 1 1 d .
Mo2 Mo 0.70225(3) 0.69181(4) 0.25069(4) 0.03293(11) Uani 1 1 d .
Mo3 Mo 0.25957(3) 0.57487(4) 0.56420(3) 0.03014(11) Uani 1 1 d .
Mo4 Mo 0.49935(3) 0.76043(4) 0.45353(4) 0.03198(11) Uani 1 1 d .
Cu1 Cu 0.75421(4) 0.79283(5) -0.11821(5) 0.03153(14) Uani 1 1 d .
O1 O 0.3579(3) 0.4487(3) 0.3153(3) 0.0440(8) Uani 1 1 d .
O2 O 0.5503(3) 0.5948(3) 0.2291(3) 0.0340(7) Uani 1 1 d .
O2W O 0.0583(6) 0.2907(5) 0.5043(5) 0.142(2) Uani 1 1 d .
H2WA H 0.0940 0.2777 0.5610 0.170 Uiso 1 1 d R
H2WB H 0.0159 0.2247 0.5222 0.170 Uiso 1 1 d R
O3 O 0.5725(3) 0.7932(3) 0.2871(3) 0.0361(7) Uani 1 1 d .
O1W O 0.7766(4) 0.8643(4) -0.3533(3) 0.0764(13) Uani 1 1 d .
H1WA H 0.8156 0.9303 -0.3905 0.092 Uiso 1 1 d R
H1WB H 0.7327 0.8591 -0.4010 0.092 Uiso 1 1 d R
O4 O 0.5983(2) 0.5764(3) 0.4450(2) 0.0278(7) Uani 1 1 d .
O5 O 0.3751(2) 0.6382(3) 0.4094(2) 0.0294(7) Uani 1 1 d .
O6 O 0.7436(3) 0.7493(3) 0.0959(3) 0.0449(9) Uani 1 1 d .
O7 O 0.4303(2) 0.6318(3) 0.6055(2) 0.0298(7) Uani 1 1 d .
O8 O 0.8027(3) 0.7448(3) 0.3048(3) 0.0457(9) Uani 1 1 d .
O9 O 0.7624(2) 0.5296(3) 0.2744(3) 0.0332(7) Uani 1 1 d .
O11 O 0.3942(3) 0.8684(3) 0.4460(3) 0.0515(9) Uani 1 1 d .
O12 O 0.1608(3) 0.5191(3) 0.5097(3) 0.0463(9) Uani 1 1 d .
O13 O 0.1962(3) 0.7040(3) 0.5854(3) 0.0445(8) Uani 1 1 d .
O14 O 0.6030(3) 0.8078(3) 0.5081(3) 0.0480(9) Uani 1 1 d .
N1 N 0.6535(4) 1.1043(4) -0.0281(4) 0.0477(11) Uani 1 1 d .
N2 N 0.7174(3) 1.1500(3) -0.1433(4) 0.0345(9) Uani 1 1 d .
N3 N 0.6986(3) 0.9595(3) -0.1162(3) 0.0340(9) Uani 1 1 d .
C13 C -0.0388(4) 0.9120(5) -0.0835(4) 0.0389(12) Uani 1 1 d .
H13B H -0.0819 0.9222 -0.0116 0.047 Uiso 1 1 calc R
N5 N 0.8133(3) 0.6263(3) -0.1076(4) 0.0335(9) Uani 1 1 d .
N6 N 0.8864(4) 0.4400(4) -0.0403(4) 0.0472(11) Uani 1 1 d .
N7 N 0.0945(3) 0.9197(3) -0.2352(3) 0.0308(8) Uani 1 1 d .
N8 N 0.5935(3) 0.7484(3) -0.1142(3) 0.0327(9) Uani 1 1 d .
N9 N 0.4220(3) 0.7523(3) -0.1585(3) 0.0282(8) Uani 1 1 d .
N10 N 0.8912(3) 0.4738(3) -0.1611(4) 0.0350(9) Uani 1 1 d .
N11 N -0.0801(3) 0.8499(3) -0.1455(3) 0.0307(8) Uani 1 1 d .
N12 N 0.4276(3) 0.6440(3) -0.0703(4) 0.0410(10) Uani 1 1 d .
C1 C 0.5327(4) 0.6470(4) -0.0489(5) 0.0390(12) Uani 1 1 d .
H1A H 0.5627 0.5836 0.0073 0.047 Uiso 1 1 calc R
C2 C 0.6432(4) 0.9899(4) -0.0161(5) 0.0438(12) Uani 1 1 d .
H2A H 0.6020 0.9346 0.0541 0.053 Uiso 1 1 calc R
C3 C 0.7640(4) 0.2731(4) -0.1904(4) 0.0386(12) Uani 1 1 d .
H3A H 0.7184 0.3221 -0.1443 0.046 Uiso 1 1 calc R
H3B H 0.7581 0.3088 -0.2747 0.046 Uiso 1 1 calc R
C4 C 0.5200(4) 0.8130(4) -0.1823(4) 0.0343(11) Uani 1 1 d .
H4A H 0.5358 0.8897 -0.2383 0.041 Uiso 1 1 calc R
C5 C 0.9449(4) 0.3955(4) -0.2329(5) 0.0464(13) Uani 1 1 d .
H5A H 1.0285 0.3886 -0.2343 0.056 Uiso 1 1 calc R
H5B H 0.9350 0.4316 -0.3159 0.056 Uiso 1 1 calc R
C6 C 0.2043(4) 0.9577(4) -0.3245(4) 0.0360(11) Uani 1 1 d .
H6A H 0.2037 1.0449 -0.3603 0.043 Uiso 1 1 calc R
H6B H 0.2087 0.9228 -0.3890 0.043 Uiso 1 1 calc R
C7 C 0.8376(4) 0.5344(4) -0.0115(5) 0.0423(12) Uani 1 1 d .
H7A H 0.8211 0.5380 0.0674 0.051 Uiso 1 1 calc R
C8 C 0.8902(4) 0.2710(4) -0.1807(4) 0.0371(11) Uani 1 1 d .
H8A H 0.9344 0.2186 -0.2235 0.045 Uiso 1 1 calc R
H8B H 0.8950 0.2377 -0.0959 0.045 Uiso 1 1 calc R
C9 C 0.8476(4) 0.5828(4) -0.2000(4) 0.0371(11) Uani 1 1 d .
H9A H 0.8417 0.6232 -0.2798 0.045 Uiso 1 1 calc R
C10 C 0.7427(4) 1.0639(4) -0.1936(5) 0.0395(12) Uani 1 1 d .
H10A H 0.7855 1.0747 -0.2722 0.047 Uiso 1 1 calc R
C11 C 0.3123(3) 0.9210(4) -0.2707(4) 0.0327(11) Uani 1 1 d .
H11A H 0.3820 0.9429 -0.3352 0.039 Uiso 1 1 calc R
H11B H 0.3140 0.9650 -0.2146 0.039 Uiso 1 1 calc R
C12 C 0.3149(4) 0.7870(4) -0.2045(4) 0.0333(10) Uani 1 1 d .
H12A H 0.2474 0.7656 -0.1373 0.040 Uiso 1 1 calc R
H12B H 0.3096 0.7427 -0.2594 0.040 Uiso 1 1 calc R
N4 N 0.0666(3) 0.9556(4) -0.1344(4) 0.0409(10) Uani 1 1 d .
C14 C 0.0078(4) 0.8571(4) -0.2392(4) 0.0333(11) Uani 1 1 d .
H14A H 0.0081 0.8226 -0.2995 0.040 Uiso 1 1 calc R
O3W O 0.9332(6) 1.0860(7) -0.4474(5) 0.157(3) Uani 1 1 d .
H3WA H 0.9873 1.1368 -0.4518 0.189 Uiso 1 1 d R
H3WB H 0.8835 1.1309 -0.4858 0.189 Uiso 1 1 d 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
O1 Mo1 O2 105.05(15) . .
O1 Mo1 O7 101.87(14) . 2_666
O2 Mo1 O7 96.72(13) . 2_666
O1 Mo1 O5 101.34(14) . .
O2 Mo1 O5 96.05(13) . .
O7 Mo1 O5 149.51(11) 2_666 .
O1 Mo1 O4 98.96(14) . 2_666
O2 Mo1 O4 155.96(12) . 2_666
O7 Mo1 O4 79.13(11) 2_666 2_666
O5 Mo1 O4 77.96(11) . 2_666
O1 Mo1 O4 175.44(13) . .
O2 Mo1 O4 79.47(11) . .
O7 Mo1 O4 77.88(11) 2_666 .
O5 Mo1 O4 77.42(10) . .
O4 Mo1 O4 76.50(11) 2_666 .
O8 Mo2 O6 105.30(16) . .
O8 Mo2 O3 98.83(15) . .
O6 Mo2 O3 102.48(14) . .
O8 Mo2 O9 98.16(14) . .
O6 Mo2 O9 99.70(14) . .
O3 Mo2 O9 147.28(13) . .
O8 Mo2 O2 165.35(13) . .
O6 Mo2 O2 89.30(14) . .
O3 Mo2 O2 78.66(12) . .
O9 Mo2 O2 77.85(12) . .
O8 Mo2 O4 94.66(13) . .
O6 Mo2 O4 159.91(13) . .
O3 Mo2 O4 76.21(11) . .
O9 Mo2 O4 74.71(11) . .
O2 Mo2 O4 70.71(10) . .
O12 Mo3 O13 104.34(16) . .
O12 Mo3 O9 101.57(15) . 2_666
O13 Mo3 O9 101.28(14) . 2_666
O12 Mo3 O5 97.82(14) . .
O13 Mo3 O5 101.90(14) . .
O9 Mo3 O5 144.87(12) 2_666 .
O12 Mo3 O7 165.45(13) . .
O13 Mo3 O7 87.60(13) . .
O9 Mo3 O7 83.84(11) 2_666 .
O5 Mo3 O7 71.17(11) . .
O12 Mo3 O4 96.25(13) . 2_666
O13 Mo3 O4 159.33(13) . 2_666
O9 Mo3 O4 75.96(11) 2_666 2_666
O5 Mo3 O4 73.02(10) . 2_666
O7 Mo3 O4 71.76(10) . 2_666
O11 Mo4 O14 104.85(17) . .
O11 Mo4 O3 101.45(15) . .
O14 Mo4 O3 101.78(15) . .
O11 Mo4 O7 102.19(14) . .
O14 Mo4 O7 97.15(14) . .
O3 Mo4 O7 144.62(12) . .
O11 Mo4 O5 89.78(14) . .
O14 Mo4 O5 162.96(14) . .
O3 Mo4 O5 83.39(12) . .
O7 Mo4 O5 70.79(11) . .
O11 Mo4 O4 160.32(14) . .
O14 Mo4 O4 94.73(13) . .
O3 Mo4 O4 76.01(11) . .
O7 Mo4 O4 72.86(10) . .
O5 Mo4 O4 70.56(9) . .
N8 Cu1 N5 91.92(14) . .
N8 Cu1 N11 172.51(15) . 1_655
N5 Cu1 N11 90.16(15) . 1_655
N8 Cu1 N3 90.39(14) . .
N5 Cu1 N3 175.36(15) . .
N11 Cu1 N3 88.05(15) 1_655 .
N8 Cu1 O6 99.87(14) . .
N5 Cu1 O6 90.21(13) . .
N11 Cu1 O6 87.30(13) 1_655 .
N3 Cu1 O6 85.43(13) . .
Mo1 O2 Mo2 117.03(14) . .
Mo4 O3 Mo2 116.48(15) . .
Mo1 O4 Mo3 91.85(10) 2_666 2_666
Mo1 O4 Mo2 163.67(14) 2_666 .
Mo3 O4 Mo2 87.19(9) 2_666 .
Mo1 O4 Mo1 103.50(11) 2_666 .
Mo3 O4 Mo1 97.07(10) 2_666 .
Mo2 O4 Mo1 92.79(9) . .
Mo1 O4 Mo4 90.84(9) 2_666 .
Mo3 O4 Mo4 164.23(13) 2_666 .
Mo2 O4 Mo4 85.88(9) . .
Mo1 O4 Mo4 97.40(10) . .
Mo1 O5 Mo3 110.20(14) . .
Mo1 O5 Mo4 112.02(12) . .
Mo3 O5 Mo4 103.69(12) . .
Mo2 O6 Cu1 162.87(19) . .
Mo1 O7 Mo4 110.25(13) 2_666 .
Mo1 O7 Mo3 110.79(13) 2_666 .
Mo4 O7 Mo3 103.76(12) . .
Mo3 O9 Mo2 116.97(14) 2_666 .
C2 N1 N2 102.9(4) . .
C10 N2 N1 110.0(4) . .
C10 N2 C3 127.4(4) . 1_565
N1 N2 C3 121.8(4) . 1_565
C10 N3 C2 103.0(4) . .
C10 N3 Cu1 126.9(3) . .
C2 N3 Cu1 125.9(3) . .
N4 C13 N11 113.7(4) . .
C9 N5 C7 103.2(4) . .
C9 N5 Cu1 126.2(3) . .
C7 N5 Cu1 130.5(3) . .
C7 N6 N10 102.4(4) . .
C14 N7 N4 109.8(4) . .
C14 N7 C6 128.9(4) . .
N4 N7 C6 121.1(4) . .
C4 N8 C1 103.1(4) . .
C4 N8 Cu1 127.0(3) . .
C1 N8 Cu1 129.8(3) . .
C4 N9 N12 109.6(4) . .
C4 N9 C12 130.3(4) . .
N12 N9 C12 120.0(3) . .
C9 N10 N6 111.0(4) . .
C9 N10 C5 127.9(4) . .
N6 N10 C5 121.0(4) . .
C14 N11 C13 102.9(4) . .
C14 N11 Cu1 128.6(3) . 1_455
C13 N11 Cu1 127.4(3) . 1_455
C1 N12 N9 102.6(4) . .
N12 C1 N8 114.7(4) . .
N1 C2 N3 113.8(5) . .
N2 C3 C8 109.8(4) 1_545 .
N9 C4 N8 110.1(4) . .
N10 C5 C8 111.3(4) . .
N7 C6 C11 113.1(3) . .
N6 C7 N5 113.9(4) . .
C3 C8 C5 112.2(4) . .
N10 C9 N5 109.5(4) . .
N2 C10 N3 110.3(4) . .
C12 C11 C6 112.2(4) . .
N9 C12 C11 111.5(4) . .
C13 N4 N7 103.0(4) . .
N7 C14 N11 110.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.681(3) .
Mo1 O2 1.749(3) .
Mo1 O7 1.957(3) 2_666
Mo1 O5 1.964(3) .
Mo1 O4 2.148(3) 2_666
Mo1 O4 2.387(3) .
Mo2 O8 1.695(3) .
Mo2 O6 1.712(3) .
Mo2 O3 1.915(3) .
Mo2 O9 1.929(3) .
Mo2 O2 2.276(3) .
Mo2 O4 2.369(3) .
Mo3 O12 1.701(3) .
Mo3 O13 1.701(3) .
Mo3 O9 1.886(3) 2_666
Mo3 O5 1.978(3) .
Mo3 O7 2.345(3) .
Mo3 O4 2.348(3) 2_666
Mo4 O11 1.692(3) .
Mo4 O14 1.695(3) .
Mo4 O3 1.897(3) .
Mo4 O7 1.988(3) .
Mo4 O5 2.356(3) .
Mo4 O4 2.390(3) .
Cu1 N8 1.969(3) .
Cu1 N5 1.993(4) .
Cu1 N11 2.014(3) 1_655
Cu1 N3 2.016(4) .
Cu1 O6 2.407(3) .
O4 Mo1 2.148(3) 2_666
O4 Mo3 2.348(3) 2_666
O7 Mo1 1.957(3) 2_666
O9 Mo3 1.886(3) 2_666
N1 C2 1.311(6) .
N1 N2 1.359(5) .
N2 C10 1.315(5) .
N2 C3 1.463(5) 1_565
N3 C10 1.326(6) .
N3 C2 1.364(6) .
C13 N4 1.304(6) .
C13 N11 1.364(5) .
N5 C9 1.328(5) .
N5 C7 1.360(6) .
N6 C7 1.315(6) .
N6 N10 1.352(5) .
N7 C14 1.308(5) .
N7 N4 1.362(5) .
N7 C6 1.462(5) .
N8 C4 1.335(5) .
N8 C1 1.340(6) .
N9 C4 1.318(5) .
N9 N12 1.367(5) .
N9 C12 1.454(5) .
N10 C9 1.315(6) .
N10 C5 1.464(5) .
N11 C14 1.321(5) .
N11 Cu1 2.014(3) 1_455
N12 C1 1.313(6) .
C3 N2 1.463(5) 1_545
C3 C8 1.500(6) .
C5 C8 1.513(6) .
C6 C11 1.512(6) .
C11 C12 1.512(6) .
