#------------------------------------------------------------------------------
#$Date: 2017-06-15 07:02:21 +0200 (jue 15 de jun de 2017) $
#$Revision: 197843 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/84/7228474.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_7228474
loop_
_publ_author_name
'Tian, Aixiang'
'Ni, Huaiping'
'Ji, Xuebin'
'Tian, Yan'
'Liu, Guocheng'
'Ying, Jun'
_publ_section_title
;
 Influence of pendant 2-[1,2,4]triazol-4-yl-ethylamine and symmetrical
 bis(pyrazol) ligands on dimensional extension of POM-based compounds
;
_journal_issue                   49
_journal_name_full               'RSC Adv.'
_journal_page_first              30573
_journal_paper_doi               10.1039/C7RA03884D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C8 H16 Cr0 Cu3 K2 Mo8 N8 O31'
_chemical_formula_weight         1756.63
_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
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.957(2)
_cell_angle_beta                 102.211(2)
_cell_angle_gamma                100.545(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4612(7)
_cell_length_b                   10.5659(11)
_cell_length_c                   10.7372(9)
_cell_measurement_reflns_used    3273
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.00
_cell_volume                     895.82(14)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0160
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6666
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    4.790
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       clavate
_exptl_crystal_F_000             829
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.916
_refine_diff_density_min         -2.445
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0668P)²+8.4945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                3833
_reflns_number_total             4454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra03884d2.cif
_cod_data_source_block           compound-1
_cod_database_code               7228474
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 -0.32379(7) 0.43609(5) 0.01213(5) 0.00911(13) Uani 1 1 d .
O1 O -0.3925(6) 0.5854(5) 0.1063(4) 0.0120(9) Uani 1 1 d .
N1 N 0.1278(7) 0.6548(6) 0.4438(6) 0.0155(11) Uani 1 1 d .
O15 O 0.0259(6) 0.3770(5) 0.3504(4) 0.0154(9) Uani 1 1 d .
C1 C 0.1762(9) 0.7843(7) 0.4913(7) 0.0186(14) Uani 1 1 d .
H1A H 0.1732 0.8287 0.5740 0.022 Uiso 1 1 calc R
O2 O -0.4451(6) 0.7016(5) 0.3156(5) 0.0148(9) Uani 1 1 d .
N2 N 0.1572(8) 0.6294(6) 0.3215(6) 0.0168(11) Uani 1 1 d .
N3 N 0.2306(8) 0.8429(6) 0.4017(6) 0.0181(12) Uani 1 1 d .
Mo3 Mo -0.44399(7) 0.51919(5) 0.28218(5) 0.00969(13) Uani 1 1 d .
O3 O -0.6037(6) 0.7449(5) 0.0614(4) 0.0154(9) Uani 1 1 d .
C2 C 0.2165(9) 0.7433(7) 0.2984(7) 0.0191(14) Uani 1 1 d .
H2A H 0.2449 0.7540 0.2213 0.023 Uiso 1 1 calc R
Mo4 Mo -0.33235(7) 0.80114(6) 0.20113(6) 0.01584(15) Uani 1 1 d .
O4 O -0.3682(8) 0.9479(5) 0.2750(5) 0.0276(12) Uani 1 1 d .
C3 C 0.2954(10) 0.9853(7) 0.4143(8) 0.0218(15) Uani 1 1 d .
H3A H 0.3616 0.9956 0.3517 0.026 Uiso 1 1 calc R
H3B H 0.3677 1.0242 0.5016 0.026 Uiso 1 1 calc R
Cu2 Cu 0.0000 0.5000 0.5000 0.0131(2) Uani 1 2 d S
O5 O -0.3071(7) 0.8272(5) 0.0355(5) 0.0203(11) Uani 1 1 d .
C4 C 0.1588(11) 1.0596(8) 0.3910(9) 0.0289(17) Uani 1 1 d .
H4A H 0.0900 1.0263 0.3018 0.035 Uiso 1 1 calc R
H4B H 0.0889 1.0477 0.4507 0.035 Uiso 1 1 calc R
Cu1 Cu 0.13632(10) 0.44276(8) 0.22835(8) 0.01420(18) Uani 1 1 d .
O6 O -0.5522(6) 0.6329(4) -0.1459(4) 0.0127(9) Uani 1 1 d .
N4 N 0.2404(9) 1.2048(6) 0.4139(7) 0.0256(14) Uani 1 1 d .
H4C H 0.3470 1.2307 0.4362 0.031 Uiso 1 1 calc R
H4D H 0.1802 1.2614 0.4048 0.031 Uiso 1 1 calc R
O14 O -0.5000 1.0000 0.0000 0.0207(15) Uani 1 2 d S
O8 O -0.7042(6) 0.5048(5) 0.1293(4) 0.0133(9) Uani 1 1 d .
O9 O -0.7407(7) 0.8081(5) -0.1860(6) 0.0261(12) Uani 1 1 d .
O10 O -0.2525(6) 0.5294(5) 0.3793(5) 0.0209(11) Uani 1 1 d .
O11 O -0.1331(7) 0.8072(6) 0.2780(6) 0.0325(14) Uani 1 1 d .
O12 O -0.1261(6) 0.4536(6) 0.0984(5) 0.0215(11) Uani 1 1 d .
O7 O -0.4301(8) 0.8520(6) -0.2229(6) 0.0278(12) Uani 1 1 d .
O13 O -0.5826(6) 0.4483(5) 0.3587(5) 0.0182(10) Uani 1 1 d .
Mo2 Mo -0.53652(7) 0.83044(5) -0.10727(5) 0.01231(14) Uani 1 1 d .
K1 K 0.1002(2) 0.12638(19) 0.01880(18) 0.0289(4) Uani 1 1 d .
O16 O 0.1124(8) 0.2602(6) 0.1315(7) 0.0361(15) 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'
Cr Cr 0.3209 0.6236 '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'
K K 0.2009 0.2494 '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
O12 Mo1 O8 102.6(2) . 2_465
O12 Mo1 O3 103.6(2) . 2_465
O8 Mo1 O3 100.4(2) 2_465 2_465
O12 Mo1 O1 103.4(2) . .
O8 Mo1 O1 99.7(2) 2_465 .
O3 Mo1 O1 141.6(2) 2_465 .
O12 Mo1 O6 98.5(2) . 2_465
O8 Mo1 O6 158.8(2) 2_465 2_465
O3 Mo1 O6 77.04(19) 2_465 2_465
O1 Mo1 O6 72.42(18) . 2_465
O12 Mo1 O1 178.6(2) . 2_465
O8 Mo1 O1 78.23(18) 2_465 2_465
O3 Mo1 O1 77.33(19) 2_465 2_465
O1 Mo1 O1 75.3(2) . 2_465
O6 Mo1 O1 80.66(17) 2_465 2_465
Mo1 O1 Mo4 148.0(2) . .
Mo1 O1 Mo3 103.28(19) . .
Mo4 O1 Mo3 95.07(17) . .
Mo1 O1 Mo1 104.7(2) . 2_465
Mo4 O1 Mo1 98.17(16) . 2_465
Mo3 O1 Mo1 98.20(17) . 2_465
C1 N1 N2 106.7(6) . .
C1 N1 Cu2 135.0(5) . .
N2 N1 Cu2 117.7(4) . .
Cu1 O15 Cu2 120.0(2) . .
N1 C1 N3 109.9(6) . .
Mo3 O2 Mo4 113.6(2) . .
C2 N2 N1 107.5(6) . .
C2 N2 Cu1 132.6(5) . .
N1 N2 Cu1 119.3(4) . .
C2 N3 C1 105.5(6) . .
C2 N3 C3 126.7(6) . .
C1 N3 C3 127.8(6) . .
O10 Mo3 O13 105.3(2) . .
O10 Mo3 O2 99.2(2) . .
O13 Mo3 O2 105.8(2) . .
O10 Mo3 O6 97.2(2) . 2_465
O13 Mo3 O6 100.8(2) . 2_465
O2 Mo3 O6 143.6(2) . 2_465
O10 Mo3 O1 104.5(2) . .
O13 Mo3 O1 149.7(2) . .
O2 Mo3 O1 74.62(18) . .
O6 Mo3 O1 69.86(18) 2_465 .
O10 Mo3 O8 175.1(2) . .
O13 Mo3 O8 79.1(2) . .
O2 Mo3 O8 81.30(18) . .
O6 Mo3 O8 79.81(18) 2_465 .
O1 Mo3 O8 70.87(16) . .
Mo1 O3 Mo2 103.7(2) 2_465 .
Mo1 O3 Mo4 112.0(2) 2_465 .
Mo2 O3 Mo4 97.08(19) . .
N2 C2 N3 110.4(6) . .
O11 Mo4 O4 104.2(3) . .
O11 Mo4 O5 100.8(3) . .
O4 Mo4 O5 103.5(2) . .
O11 Mo4 O2 97.4(3) . .
O4 Mo4 O2 91.9(2) . .
O5 Mo4 O2 152.3(2) . .
O11 Mo4 O1 94.8(2) . .
O4 Mo4 O1 156.8(3) . .
O5 Mo4 O1 85.6(2) . .
O2 Mo4 O1 72.14(18) . .
O11 Mo4 O3 166.0(3) . .
O4 Mo4 O3 89.6(2) . .
O5 Mo4 O3 74.0(2) . .
O2 Mo4 O3 83.33(18) . .
O1 Mo4 O3 72.12(16) . .
O11 Mo4 K1 74.7(2) . 2_565
O4 Mo4 K1 106.5(2) . 2_565
O5 Mo4 K1 26.32(16) . 2_565
O2 Mo4 K1 161.12(14) . 2_565
O1 Mo4 K1 91.16(12) . 2_565
O3 Mo4 K1 100.22(12) . 2_565
N3 C3 C4 112.8(6) . .
O15 Cu2 O15 180.0(2) . 2_566
O15 Cu2 N1 89.7(2) . .
O15 Cu2 N1 90.3(2) 2_566 .
O15 Cu2 N1 90.3(2) . 2_566
O15 Cu2 N1 89.7(2) 2_566 2_566
N1 Cu2 N1 180.000(1) . 2_566
O15 Cu2 O10 92.54(19) . .
O15 Cu2 O10 87.46(19) 2_566 .
N1 Cu2 O10 89.8(2) . .
N1 Cu2 O10 90.2(2) 2_566 .
O15 Cu2 O10 87.46(19) . 2_566
O15 Cu2 O10 92.54(19) 2_566 2_566
N1 Cu2 O10 90.2(2) . 2_566
N1 Cu2 O10 89.8(2) 2_566 2_566
O10 Cu2 O10 180.000(1) . 2_566
Mo4 O5 K1 128.3(3) . 2_565
Mo4 O5 Mo2 116.1(2) . .
K1 O5 Mo2 115.1(2) 2_565 .
N4 C4 C3 107.9(7) . .
O15 Cu1 O16 89.9(3) . .
O15 Cu1 O8 166.9(2) . 1_655
O16 Cu1 O8 89.1(2) . 1_655
O15 Cu1 N2 91.1(2) . .
O16 Cu1 N2 178.2(3) . .
O8 Cu1 N2 90.2(2) 1_655 .
O15 Cu1 O12 89.64(19) . .
O16 Cu1 O12 91.7(2) . .
O8 Cu1 O12 103.42(19) 1_655 .
N2 Cu1 O12 86.9(2) . .
O15 Cu1 K1 96.47(15) . .
O16 Cu1 K1 6.9(2) . .
O8 Cu1 K1 83.29(14) 1_655 .
N2 Cu1 K1 171.51(17) . .
O12 Cu1 K1 89.33(14) . .
Mo3 O6 Mo2 143.4(2) 2_465 .
Mo3 O6 Mo1 108.3(2) 2_465 2_465
Mo2 O6 Mo1 105.07(19) . 2_465
Mo2 O14 Mo2 180.00(4) . 2_475
Mo1 O8 Cu1 146.6(3) 2_465 1_455
Mo1 O8 Mo3 112.6(2) 2_465 .
Cu1 O8 Mo3 100.54(18) 1_455 .
Mo3 O10 Cu2 169.2(3) . .
Mo1 O12 Cu1 170.2(3) . .
Mo2 O7 K1 89.6(2) . 2_565
O7 Mo2 O9 105.2(3) . .
O7 Mo2 O14 104.9(2) . .
O9 Mo2 O14 99.63(19) . .
O7 Mo2 O6 92.7(2) . .
O9 Mo2 O6 92.0(2) . .
O14 Mo2 O6 155.42(13) . .
O7 Mo2 O5 91.4(2) . .
O9 Mo2 O5 162.2(2) . .
O14 Mo2 O5 81.91(14) . .
O6 Mo2 O5 80.54(19) . .
O7 Mo2 O3 155.9(2) . .
O9 Mo2 O3 92.2(2) . .
O14 Mo2 O3 88.26(12) . .
O6 Mo2 O3 69.62(17) . .
O5 Mo2 O3 70.07(18) . .
O7 Mo2 K1 61.5(2) . 2_565
O9 Mo2 K1 166.6(2) . 2_565
O14 Mo2 K1 86.25(4) . 2_565
O6 Mo2 K1 87.22(14) . 2_565
O5 Mo2 K1 30.28(13) . 2_565
O3 Mo2 K1 100.12(13) . 2_565
O16 K1 O5 102.2(3) . 2_565
O16 K1 K1 127.2(3) . 2
O5 K1 K1 127.6(2) 2_565 2
O16 K1 O7 77.2(3) . 2_565
O5 K1 O7 63.21(19) 2_565 2_565
K1 K1 O7 107.71(14) 2 2_565
O16 K1 Mo4 111.3(2) . 2_565
O5 K1 Mo4 25.35(15) 2_565 2_565
K1 K1 Mo4 121.23(9) 2 2_565
O7 K1 Mo4 88.53(11) 2_565 2_565
O16 K1 Mo2 91.1(2) . 2_565
O5 K1 Mo2 34.58(15) 2_565 2_565
K1 K1 Mo2 118.72(10) 2 2_565
O7 K1 Mo2 28.87(10) 2_565 2_565
Mo4 K1 Mo2 59.77(3) 2_565 2_565
O16 K1 Cu1 8.3(3) . .
O5 K1 Cu1 97.10(17) 2_565 .
K1 K1 Cu1 133.89(10) 2 .
O7 K1 Cu1 80.32(11) 2_565 .
Mo4 K1 Cu1 103.97(5) 2_565 .
Mo2 K1 Cu1 90.50(4) 2_565 .
K1 O16 Cu1 164.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O12 1.690(5) .
Mo1 O8 1.792(4) 2_465
Mo1 O3 1.857(5) 2_465
Mo1 O1 1.957(4) .
Mo1 O6 2.109(5) 2_465
Mo1 O1 2.414(5) 2_465
O1 Mo4 2.228(5) .
O1 Mo3 2.233(4) .
O1 Mo1 2.414(5) 2_465
N1 C1 1.320(9) .
N1 N2 1.373(7) .
N1 Cu2 2.052(6) .
O15 Cu1 1.924(5) .
O15 Cu2 1.943(5) .
C1 N3 1.353(9) .
O2 Mo3 1.894(5) .
O2 Mo4 2.037(5) .
N2 C2 1.307(9) .
N2 Cu1 1.992(6) .
N3 C2 1.344(9) .
N3 C3 1.474(9) .
Mo3 O10 1.704(5) .
Mo3 O13 1.713(5) .
Mo3 O6 1.948(4) 2_465
Mo3 O8 2.413(5) .
O3 Mo1 1.857(5) 2_465
O3 Mo2 2.300(5) .
O3 Mo4 2.362(5) .
Mo4 O11 1.697(6) .
Mo4 O4 1.712(5) .
Mo4 O5 1.900(5) .
Mo4 K1 3.4813(19) 2_565
C3 C4 1.517(11) .
Cu2 O15 1.943(5) 2_566
Cu2 N1 2.052(6) 2_566
Cu2 O10 2.359(5) .
Cu2 O10 2.359(5) 2_566
O5 K1 1.967(5) 2_565
O5 Mo2 2.214(5) .
C4 N4 1.512(10) .
Cu1 O16 1.962(6) .
Cu1 O8 1.982(5) 1_655
Cu1 O12 2.394(5) .
Cu1 K1 3.579(2) .
O6 Mo3 1.948(4) 2_465
O6 Mo2 2.022(4) .
O6 Mo1 2.109(5) 2_465
O14 Mo2 1.8693(6) .
O14 Mo2 1.8693(6) 2_475
O8 Mo1 1.792(4) 2_465
O8 Cu1 1.982(5) 1_455
O9 Mo2 1.707(6) .
O7 Mo2 1.706(5) .
O7 K1 3.104(7) 2_565
Mo2 K1 3.5318(19) 2_565
K1 O16 1.648(6) .
K1 O5 1.967(5) 2_565
K1 K1 2.795(4) 2
K1 O7 3.104(7) 2_565
K1 Mo4 3.4813(19) 2_565
K1 Mo2 3.5318(19) 2_565
