#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:38:20 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705288.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_7705288
loop_
_publ_author_name
'Qu, Di'
'Liu, Xiaoting'
'Duan, Fengxue'
'Xue, Rong'
'Li, Bao'
'Wu, Lixin'
_publ_section_title
;
{VMo9O31[RC(CH2O)3]}6-:
the first class of triol ligand covalently-decorated Keggin-type
polyoxomolybdates.
;
_journal_issue 37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 12950
_journal_page_last 12954
_journal_paper_doi 10.1039/d0dt02506b
_journal_volume 49
_journal_year 2020
_chemical_formula_moiety 'C5 H9 Mo9 O34 V, 9(H2 O), 6(N H4)'
_chemical_formula_sum 'C5 H51 Mo9 N6 O43 V'
_chemical_formula_weight 1797.92
_space_group_crystal_system orthorhombic
_space_group_IT_number 36
_space_group_name_Hall 'C 2c -2'
_space_group_name_H-M_alt 'C m c 21'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2014/7
_audit_update_record
;
2020-08-06 deposited with the CCDC. 2020-08-27 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 13.858(5)
_cell_length_b 15.952(4)
_cell_length_c 20.649(5)
_cell_measurement_reflns_used 9721
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.48
_cell_measurement_theta_min 2.77
_cell_volume 4565(2)
_computing_cell_refinement 'Bruker D8 Venture'
_computing_data_collection 'Bruker D8 Venture'
_computing_data_reduction 'Bruker D8 Venture'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution 'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'D8 VENTURE PHOTON II'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0234
_diffrn_reflns_av_unetI/netI 0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 28379
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.518
_diffrn_reflns_theta_min 2.772
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 2.699
_exptl_absorpt_correction_T_max 0.774
_exptl_absorpt_correction_T_min 0.720
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS; Bruker, 2014'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.616
_exptl_crystal_description block
_exptl_crystal_F_000 3472
_exptl_crystal_size_max 0.130
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.100
_refine_diff_density_max 1.005
_refine_diff_density_min -0.497
_refine_diff_density_rms 0.094
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.17(4)
_refine_ls_extinction_coef 0.00059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref 1.141
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 313
_refine_ls_number_reflns 5411
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.141
_refine_ls_R_factor_all 0.0170
_refine_ls_R_factor_gt 0.0168
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+5.7710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0488
_refine_ls_wR_factor_ref 0.0489
_reflns_Friedel_coverage 0.947
_reflns_Friedel_fraction_full 0.998
_reflns_Friedel_fraction_max 0.997
_reflns_number_gt 5378
_reflns_number_total 5411
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0dt02506b2.cif
_cod_data_source_block mo_LXT0704_5_0m
_cod_depositor_comments
'Adding full bibliography for 7705288--7705290.cif.'
_cod_database_code 7705288
_shelx_shelxl_version_number 2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.720
_shelx_estimated_absorpt_t_max 0.774
_shelx_res_file
;
mo_LXT0704_5_0m.res created by SHELXL-2014/7
TITL mo_LXT0704_5_0m_a.res in Cmc2(1)
CELL 0.71073 13.8577 15.9522 20.6489 90 90 90
ZERR 4 0.0045 0.0042 0.0047 0 0 0
LATT -7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,+Z
SYMM +X,-Y,0.5+Z
SFAC C H N O V Mo
UNIT 20 204 24 172 4 36
L.S. 6
PLAN -8
SIZE 0.1 0.12 0.13
TEMP 20
BOND $H
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 2 0 -6
OMIT 0 4 0
OMIT 2 0 6
OMIT 2 2 0
OMIT 1 3 2
OMIT 1 5 0
OMIT 1 3 -2
OMIT 1 3 0
OMIT 2 0 0
REM
REM
REM
WGHT 0.027400 5.771000
EXTI 0.000587
BASF 0.17269
FVAR 0.08900
C1 1 0.500000 0.395483 0.625665 10.50000 0.02392 0.02182 =
0.01824 0.00726 0.00000 0.00000
AFIX 23
H1A 2 0.443474 0.390267 0.653077 10.50000 -1.20000
H1B 2 0.556526 0.390267 0.653077 10.50000 -1.20000
AFIX 0
C2 1 0.590689 0.327082 0.534737 11.00000 0.02291 0.01681 =
0.02955 0.00415 -0.00141 0.00289
AFIX 23
H2A 2 0.646902 0.322168 0.562470 11.00000 -1.20000
H2B 2 0.590695 0.279594 0.505397 11.00000 -1.20000
AFIX 0
C3 1 0.500000 0.323757 0.576442 10.50000 0.02465 0.01384 =
0.02324 0.00514 0.00000 0.00000
C4 1 0.500000 0.241661 0.613025 10.50000 0.03816 0.02068 =
0.04455 0.01195 0.00000 0.00000
AFIX 137
H4A 2 0.456259 0.245337 0.648965 10.50000 -1.50000
H4B 2 0.563876 0.230200 0.628691 10.50000 -1.50000
H4C 2 0.479865 0.197316 0.584648 10.50000 -1.50000
AFIX 0
MO1 6 0.621020 0.756138 0.561122 11.00000 0.02549 0.01741 =
0.01911 -0.00269 -0.00105 -0.00441
MO2 6 0.758197 0.651594 0.424255 11.00000 0.02137 0.02267 =
0.02163 -0.00034 0.00368 -0.00558
MO3 6 0.636690 0.563521 0.301201 11.00000 0.02837 0.02569 =
0.01616 -0.00265 0.00420 -0.00123
MO4 6 0.628234 0.517957 0.548266 11.00000 0.01636 0.01592 =
0.01694 0.00023 -0.00084 -0.00134
MO5 6 0.500000 0.421981 0.417741 10.50000 0.02130 0.01577 =
0.01678 -0.00204 0.00000 0.00000
N1 3 1.000000 0.884867 0.207797 10.50000 0.04080 0.04141 =
0.02796 -0.00190 0.00000 0.00000
AFIX 3
H1C 2 1.030130 0.877158 0.170208 10.50000 -1.20000
H1D 2 0.979420 0.937608 0.210397 10.50000 -1.20000
H1E 2 1.041540 0.874258 0.240937 10.50000 -1.20000
H1F 2 0.948700 0.849418 0.210457 10.50000 -1.20000
AFIX 0
N2 3 0.500000 0.162763 0.336678 10.50000 0.07128 0.05481 =
0.07523 -0.01106 0.00000 0.00000
AFIX 3
H2C 2 0.552440 0.134153 0.348117 10.50000 -1.20000
H2D 2 0.447560 0.134153 0.348117 10.50000 -1.20000
H2E 2 0.500000 0.213415 0.356928 10.50000 -1.20000
H2F 2 0.500000 0.170593 0.293017 10.50000 -1.20000
AFIX 0
N3 3 0.714375 0.899117 0.410230 11.00000 0.05464 0.03115 =
0.04782 0.00350 0.01136 -0.00628
AFIX 3
H3A 2 0.677385 0.883237 0.377200 11.00000 -1.20000
H3B 2 0.724245 0.954197 0.408210 11.00000 -1.20000
H3C 2 0.770745 0.872527 0.408210 11.00000 -1.20000
H3D 2 0.684455 0.886257 0.448178 11.00000 -1.20000
AFIX 0
O24 4 0.599635 0.033603 0.569332 11.00000 0.04235 0.05164 =
0.06369 0.00109 0.01322 0.00417
AFIX 3
H24A 2 0.607856 0.062096 0.535059 11.00000 -1.50000
H24B 2 0.601943 -0.017787 0.558828 11.00000 -1.50000
AFIX 0
O1 4 0.500000 0.757636 0.607346 10.50000 0.02913 0.02135 =
0.01567 -0.00513 0.00000 0.00000
O2 4 0.699766 0.761815 0.625013 11.00000 0.03359 0.03472 =
0.02849 -0.00526 -0.00431 -0.00820
O3 4 0.616361 0.857529 0.532568 11.00000 0.04494 0.01769 =
0.03760 0.00039 0.00279 -0.00256
O4 4 0.700888 0.712171 0.494240 11.00000 0.02622 0.02232 =
0.02482 -0.00291 0.00234 -0.00632
O5 4 0.500000 0.720717 0.489510 10.50000 0.02616 0.01693 =
0.01907 -0.00299 0.00000 0.00000
O6 4 0.608675 0.619275 0.581016 11.00000 0.02565 0.02091 =
0.02055 -0.00059 0.00235 -0.00384
O7 4 0.872269 0.630052 0.452504 11.00000 0.02479 0.04084 =
0.03798 -0.00099 0.00107 -0.00537
O8 4 0.776091 0.736097 0.374606 11.00000 0.04255 0.03072 =
0.02999 0.00195 0.00953 -0.00872
O9 4 0.750711 0.567725 0.356679 11.00000 0.02564 0.02639 =
0.02299 -0.00178 0.00451 -0.00062
O10 4 0.705446 0.546683 0.483429 11.00000 0.02444 0.02166 =
0.02319 -0.00003 0.00304 -0.00214
O11 4 0.659144 0.654161 0.259615 11.00000 0.04247 0.03890 =
0.02662 0.00540 0.00217 -0.00638
O12 4 0.673714 0.486707 0.249716 11.00000 0.03888 0.03910 =
0.02786 -0.01123 0.00816 -0.00174
O13 4 0.500000 0.558800 0.289943 10.50000 0.03290 0.03303 =
0.01772 0.00091 0.00000 0.00000
O14 4 0.701809 0.468366 0.602220 11.00000 0.02302 0.02665 =
0.02614 0.00337 -0.00436 0.00154
O15 4 0.500000 0.543463 0.479468 10.50000 0.01930 0.01518 =
0.01341 0.00136 0.00000 0.00000
O16 4 0.500000 0.477615 0.596229 10.50000 0.01878 0.01639 =
0.01795 0.00058 0.00000 0.00000
O17 4 0.598154 0.404121 0.497128 11.00000 0.02006 0.01521 =
0.01945 0.00069 0.00010 0.00037
O18 4 0.400273 0.645030 0.389389 11.00000 0.02542 0.02195 =
0.01670 -0.00111 -0.00234 0.00372
O19 4 0.402884 0.465853 0.373603 11.00000 0.02705 0.02418 =
0.02053 0.00014 -0.00344 0.00021
O20 4 0.500000 0.318225 0.398792 10.50000 0.03379 0.02442 =
0.03028 -0.00339 0.00000 0.00000
O21 4 0.863155 0.764982 0.256937 11.00000 0.08454 0.12373 =
0.04131 0.01327 0.01025 -0.03962
AFIX 3
H21A 2 0.809055 0.746461 0.243847 11.00000 -1.50000
H21B 2 0.870895 0.810672 0.236417 11.00000 -1.50000
AFIX 0
O22 4 0.500000 0.936826 0.422121 10.50000 0.06622 0.42774 =
0.21101 0.14642 0.00000 0.00000
AFIX 3
H22A 2 0.449870 0.906986 0.416491 10.50000 -1.50000
H22B 2 0.522720 0.920446 0.458211 10.50000 -1.50000
AFIX 0
O23 4 0.897388 0.676139 0.790560 11.00000 0.07719 0.03752 =
0.08782 -0.00339 0.00810 0.00133
AFIX 3
H23A 2 0.858382 0.704080 0.799451 11.00000 -1.50000
H23B 2 0.912195 0.716598 0.790391 11.00000 -1.50000
AFIX 0
N4 3 0.801115 0.617287 0.677123 11.00000 0.03338 0.03856 =
0.04575 0.00828 0.00726 -0.00419
AFIX 3
H4D 2 0.823095 0.585907 0.644683 11.00000 -1.20000
H4E 2 0.850425 0.634527 0.701311 11.00000 -1.20000
H4F 2 0.760825 0.587157 0.701311 11.00000 -1.20000
AFIX 3
H4G 2 0.769385 0.662557 0.660822 11.00000 -1.20000
AFIX 0
O25 4 0.630052 0.919698 0.697061 11.00000 0.28302 0.12095 =
0.13281 0.00192 0.03999 -0.02855
AFIX 3
H25A 2 0.691662 0.897967 0.715900 11.00000 -1.50000
H25B 2 0.629732 0.883967 0.666510 11.00000 -1.50000
AFIX 0
V1 5 0.500000 0.640838 0.436061 10.50000 0.01932 0.01435 =
0.01450 -0.00057 0.00000 0.00000
HKLF 4
REM mo_LXT0704_5_0m_a.res in Cmc2(1)
REM R1 = 0.0168 for 5378 Fo > 4sig(Fo) and 0.0170 for all 5411 data
REM 313 parameters refined using 1 restraints
END
WGHT 0.0275 5.6494
REM Highest difference peak 1.005, deepest hole -0.497, 1-sigma level 0.094
Q1 1 0.0880 0.5116 0.3004 11.00000 0.05 1.00
Q2 1 0.0000 0.5013 0.2959 10.50000 0.05 0.81
Q3 1 0.5000 0.9592 0.4315 10.50000 0.05 0.73
Q4 1 0.5000 0.8975 0.6723 10.50000 0.05 0.44
Q5 1 0.5000 0.3579 0.4232 10.50000 0.05 0.41
Q6 1 0.5000 0.7228 0.4324 10.50000 0.05 0.39
Q7 1 0.4710 0.0295 0.5666 11.00000 0.05 0.38
Q8 1 0.7669 0.9320 0.4384 11.00000 0.05 0.37
;
_shelx_res_checksum 7626
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5000 0.3955(4) 0.6257(3) 0.0213(12) Uani 1 2 d S T P . .
H1A H 0.4435 0.3903 0.6531 0.026 Uiso 0.5 1 calc R U P . .
H1B H 0.5565 0.3903 0.6531 0.026 Uiso 0.5 1 calc R U P . .
C2 C 0.5907(3) 0.3271(3) 0.5347(2) 0.0231(9) Uani 1 1 d . . . . .
H2A H 0.6469 0.3222 0.5625 0.028 Uiso 1 1 calc R U . . .
H2B H 0.5907 0.2796 0.5054 0.028 Uiso 1 1 calc R U . . .
C3 C 0.5000 0.3238(4) 0.5764(3) 0.0206(12) Uani 1 2 d S T P . .
C4 C 0.5000 0.2417(4) 0.6130(4) 0.0345(17) Uani 1 2 d S T P . .
H4A H 0.4563 0.2453 0.6490 0.052 Uiso 0.5 1 calc R U P . .
H4B H 0.5639 0.2302 0.6287 0.052 Uiso 0.5 1 calc R U P . .
H4C H 0.4799 0.1973 0.5846 0.052 Uiso 0.5 1 calc R U P . .
Mo1 Mo 0.62102(3) 0.75614(2) 0.56112(2) 0.02067(10) Uani 1 1 d . . . . .
Mo2 Mo 0.75820(3) 0.65159(2) 0.42426(2) 0.02189(9) Uani 1 1 d . . . . .
Mo3 Mo 0.63669(3) 0.56352(3) 0.30120(2) 0.02341(10) Uani 1 1 d . . . . .
Mo4 Mo 0.62823(2) 0.51796(2) 0.54827(2) 0.01641(9) Uani 1 1 d . . . . .
Mo5 Mo 0.5000 0.42198(3) 0.41774(3) 0.01795(11) Uani 1 2 d S T P . .
N1 N 1.0000 0.8849(5) 0.2078(3) 0.0367(15) Uani 1 2 d S T P . .
H1C H 1.0301 0.8772 0.1702 0.044 Uiso 0.5 1 d R U P . .
H1D H 0.9794 0.9376 0.2104 0.044 Uiso 0.5 1 d R U P . .
H1E H 1.0415 0.8743 0.2409 0.044 Uiso 0.5 1 d R U P . .
H1F H 0.9487 0.8494 0.2105 0.044 Uiso 0.5 1 d R U P . .
N2 N 0.5000 0.1628(6) 0.3367(5) 0.067(3) Uani 1 2 d S T P . .
H2C H 0.5524 0.1342 0.3481 0.081 Uiso 0.5 1 d R U P . .
H2D H 0.4476 0.1342 0.3481 0.081 Uiso 0.5 1 d R U P . .
H2E H 0.5000 0.2134 0.3569 0.081 Uiso 1 2 d R U P . .
H2F H 0.5000 0.1706 0.2930 0.081 Uiso 1 2 d R U P . .
N3 N 0.7144(4) 0.8991(3) 0.4102(3) 0.0445(13) Uani 1 1 d . . . . .
H3A H 0.6774 0.8832 0.3772 0.053 Uiso 1 1 d R U . . .
H3B H 0.7242 0.9542 0.4082 0.053 Uiso 1 1 d R U . . .
H3C H 0.7707 0.8725 0.4082 0.053 Uiso 1 1 d R U . . .
H3D H 0.6845 0.8863 0.4482 0.053 Uiso 1 1 d R U . . .
O24 O 0.5996(3) 0.0336(3) 0.5693(3) 0.0526(11) Uani 1 1 d . . . . .
H24A H 0.6079 0.0621 0.5351 0.079 Uiso 1 1 d R U . . .
H24B H 0.6019 -0.0178 0.5588 0.079 Uiso 1 1 d R U . . .
O1 O 0.5000 0.7576(3) 0.6073(2) 0.0220(9) Uani 1 2 d S T P . .
O2 O 0.6998(3) 0.7618(2) 0.62501(18) 0.0323(8) Uani 1 1 d . . . . .
O3 O 0.6164(3) 0.8575(2) 0.5326(2) 0.0334(9) Uani 1 1 d . . . . .
O4 O 0.7009(2) 0.7122(2) 0.49424(16) 0.0245(7) Uani 1 1 d . . . . .
O5 O 0.5000 0.7207(3) 0.4895(2) 0.0207(9) Uani 1 2 d S T P . .
O6 O 0.6087(2) 0.6193(2) 0.58102(15) 0.0224(6) Uani 1 1 d . . . . .
O7 O 0.8723(2) 0.6301(3) 0.4525(2) 0.0345(8) Uani 1 1 d . . . . .
O8 O 0.7761(3) 0.7361(2) 0.37461(18) 0.0344(8) Uani 1 1 d . . . . .
O9 O 0.7507(2) 0.5677(2) 0.35668(16) 0.0250(7) Uani 1 1 d . . . . .
O10 O 0.7054(2) 0.5467(2) 0.48343(15) 0.0231(6) Uani 1 1 d . . . . .
O11 O 0.6591(3) 0.6542(2) 0.25961(19) 0.0360(8) Uani 1 1 d . . . . .
O12 O 0.6737(3) 0.4867(2) 0.24972(18) 0.0353(8) Uani 1 1 d . . . . .
O13 O 0.5000 0.5588(3) 0.2899(2) 0.0279(10) Uani 1 2 d S T P . .
O14 O 0.7018(2) 0.4684(2) 0.60222(16) 0.0253(7) Uani 1 1 d . . . . .
O15 O 0.5000 0.5435(3) 0.47947(19) 0.0160(8) Uani 1 2 d S T P . .
O16 O 0.5000 0.4776(2) 0.5962(2) 0.0177(8) Uani 1 2 d S T P . .
O17 O 0.5982(2) 0.40412(18) 0.49713(15) 0.0182(6) Uani 1 1 d . . . . .
O18 O 0.4003(2) 0.64503(19) 0.38939(15) 0.0214(6) Uani 1 1 d . . . . .
O19 O 0.4029(2) 0.4659(2) 0.37360(15) 0.0239(6) Uani 1 1 d . . . . .
O20 O 0.5000 0.3182(3) 0.3988(2) 0.0295(10) Uani 1 2 d S T P . .
O21 O 0.8632(5) 0.7650(5) 0.2569(3) 0.083(2) Uani 1 1 d . . . . .
H21A H 0.8091 0.7465 0.2438 0.125 Uiso 1 1 d R U . . .
H21B H 0.8709 0.8107 0.2364 0.125 Uiso 1 1 d R U . . .
O22 O 0.5000 0.9368(16) 0.4221(11) 0.235(12) Uani 1 2 d S T P . .
H22A H 0.4499 0.9070 0.4165 0.352 Uiso 0.5 1 d R U P . .
H22B H 0.5227 0.9204 0.4582 0.352 Uiso 0.5 1 d R U P . .
O23 O 0.8974(4) 0.6761(3) 0.7906(3) 0.0675(15) Uani 1 1 d . . . . .
H23A H 0.8584 0.7041 0.7995 0.101 Uiso 1 1 d R U . . .
H23B H 0.9122 0.7166 0.7904 0.101 Uiso 1 1 d R U . . .
N4 N 0.8011(4) 0.6173(3) 0.6771(3) 0.0392(11) Uani 1 1 d . . . . .
H4D H 0.8231 0.5859 0.6447 0.047 Uiso 1 1 d R U . . .
H4E H 0.8504 0.6345 0.7013 0.047 Uiso 1 1 d R U . . .
H4F H 0.7608 0.5872 0.7013 0.047 Uiso 1 1 d R U . . .
H4G H 0.7694 0.6626 0.6608 0.047 Uiso 1 1 d R U . . .
O25 O 0.6301(10) 0.9197(7) 0.6971(6) 0.179(6) Uani 1 1 d . . . . .
H25A H 0.6917 0.8980 0.7159 0.268 Uiso 1 1 d R U . . .
H25B H 0.6297 0.8840 0.6665 0.268 Uiso 1 1 d R U . . .
V1 V 0.5000 0.64084(6) 0.43606(5) 0.0161(2) Uani 1 2 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.024(3) 0.022(3) 0.018(3) 0.007(2) 0.000 0.000
C2 0.023(2) 0.017(2) 0.030(2) 0.0042(17) -0.0014(18) 0.0029(16)
C3 0.025(3) 0.014(3) 0.023(3) 0.005(2) 0.000 0.000
C4 0.038(4) 0.021(3) 0.045(4) 0.012(3) 0.000 0.000
Mo1 0.02549(18) 0.01741(18) 0.01911(19) -0.00269(14) -0.00105(14) -0.00441(13)
Mo2 0.02137(17) 0.02267(16) 0.02163(18) -0.00034(16) 0.00368(15) -0.00558(14)
Mo3 0.02837(19) 0.0257(2) 0.01616(18) -0.00265(16) 0.00420(15) -0.00123(15)
Mo4 0.01636(16) 0.01592(17) 0.01694(18) 0.00023(14) -0.00084(13) -0.00134(11)
Mo5 0.0213(2) 0.0158(2) 0.0168(2) -0.0020(2) 0.000 0.000
N1 0.041(4) 0.041(4) 0.028(3) -0.002(3) 0.000 0.000
N2 0.071(6) 0.055(5) 0.075(7) -0.011(5) 0.000 0.000
N3 0.055(3) 0.031(2) 0.048(3) 0.003(2) 0.011(3) -0.006(2)
O24 0.042(2) 0.052(3) 0.064(3) 0.001(2) 0.013(2) 0.004(2)
O1 0.029(2) 0.021(2) 0.016(2) -0.0051(16) 0.000 0.000
O2 0.0336(19) 0.0347(19) 0.0285(17) -0.0053(15) -0.0043(15) -0.0082(15)
O3 0.045(2) 0.0177(17) 0.038(2) 0.0004(14) 0.0028(16) -0.0026(14)
O4 0.0262(16) 0.0223(15) 0.0248(16) -0.0029(13) 0.0023(13) -0.0063(13)
O5 0.026(2) 0.017(2) 0.019(2) -0.0030(17) 0.000 0.000
O6 0.0257(15) 0.0209(15) 0.0206(16) -0.0006(13) 0.0023(13) -0.0038(13)
O7 0.0248(18) 0.041(2) 0.038(2) -0.0010(17) 0.0011(15) -0.0054(14)
O8 0.043(2) 0.0307(19) 0.0300(19) 0.0019(15) 0.0095(16) -0.0087(16)
O9 0.0256(16) 0.0264(17) 0.0230(15) -0.0018(13) 0.0045(13) -0.0006(13)
O10 0.0244(16) 0.0217(15) 0.0232(16) 0.0000(13) 0.0030(12) -0.0021(12)
O11 0.042(2) 0.039(2) 0.0266(18) 0.0054(15) 0.0022(16) -0.0064(17)
O12 0.039(2) 0.039(2) 0.0279(18) -0.0112(16) 0.0082(16) -0.0017(16)
O13 0.033(2) 0.033(3) 0.018(2) 0.0009(19) 0.000 0.000
O14 0.0230(16) 0.0266(17) 0.0261(16) 0.0034(13) -0.0044(13) 0.0015(13)
O15 0.019(2) 0.0152(19) 0.0134(19) 0.0014(16) 0.000 0.000
O16 0.019(2) 0.016(2) 0.0180(19) 0.0006(16) 0.000 0.000
O17 0.0201(14) 0.0152(14) 0.0194(14) 0.0007(11) 0.0001(11) 0.0004(11)
O18 0.0254(16) 0.0220(15) 0.0167(14) -0.0011(12) -0.0023(12) 0.0037(12)
O19 0.0271(16) 0.0242(16) 0.0205(15) 0.0001(13) -0.0034(13) 0.0002(13)
O20 0.034(3) 0.024(2) 0.030(3) -0.003(2) 0.000 0.000
O21 0.085(4) 0.124(6) 0.041(3) 0.013(3) 0.010(3) -0.040(4)
O22 0.066(8) 0.43(4) 0.211(17) 0.15(2) 0.000 0.000
O23 0.077(3) 0.038(2) 0.088(4) -0.003(3) 0.008(3) 0.001(2)
N4 0.033(2) 0.039(2) 0.046(3) 0.008(2) 0.007(2) -0.004(2)
O25 0.283(18) 0.121(8) 0.133(10) 0.002(8) 0.040(10) -0.029(8)
V1 0.0193(5) 0.0143(4) 0.0145(5) -0.0006(4) 0.000 0.000
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'
V V 0.3005 0.5294 '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
_geom_angle_publ_flag
O16 C1 C3 113.5(5) . . ?
O16 C1 H1A 108.9 . . ?
C3 C1 H1A 108.9 . . ?
O16 C1 H1B 108.9 . . ?
C3 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O17 C2 C3 112.9(4) . . ?
O17 C2 H2A 109.0 . . ?
C3 C2 H2A 109.0 . . ?
O17 C2 H2B 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 C2 108.2(3) . . ?
C4 C3 C2 108.2(3) . 3_655 ?
C2 C3 C2 111.1(5) . 3_655 ?
C4 C3 C1 108.4(5) . . ?
C2 C3 C1 110.4(3) . . ?
C2 C3 C1 110.4(3) 3_655 . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 Mo1 O3 103.75(19) . . ?
O2 Mo1 O4 101.98(16) . . ?
O3 Mo1 O4 96.86(17) . . ?
O2 Mo1 O1 99.90(17) . . ?
O3 Mo1 O1 97.19(19) . . ?
O4 Mo1 O1 150.30(15) . . ?
O2 Mo1 O6 87.64(15) . . ?
O3 Mo1 O6 168.57(16) . . ?
O4 Mo1 O6 79.48(13) . . ?
O1 Mo1 O6 81.62(16) . . ?
O2 Mo1 O5 165.74(17) . . ?
O3 Mo1 O5 89.04(18) . . ?
O4 Mo1 O5 82.38(13) . . ?
O1 Mo1 O5 71.83(14) . . ?
O6 Mo1 O5 79.76(14) . . ?
O8 Mo2 O7 103.14(19) . . ?
O8 Mo2 O4 96.60(17) . . ?
O7 Mo2 O4 103.09(17) . . ?
O8 Mo2 O9 96.91(17) . . ?
O7 Mo2 O9 98.95(18) . . ?
O4 Mo2 O9 150.71(14) . . ?
O8 Mo2 O10 168.85(16) . . ?
O7 Mo2 O10 87.99(16) . . ?
O4 Mo2 O10 80.00(13) . . ?
O9 Mo2 O10 81.76(13) . . ?
O8 Mo2 O18 89.24(16) . 3_655 ?
O7 Mo2 O18 165.73(16) . 3_655 ?
O4 Mo2 O18 82.17(13) . 3_655 ?
O9 Mo2 O18 72.16(13) . 3_655 ?
O10 Mo2 O18 79.79(12) . 3_655 ?
O12 Mo3 O11 103.90(19) . . ?
O12 Mo3 O13 101.2(2) . . ?
O11 Mo3 O13 98.8(2) . . ?
O12 Mo3 O9 98.47(17) . . ?
O11 Mo3 O9 96.79(17) . . ?
O13 Mo3 O9 151.07(17) . . ?
O12 Mo3 O19 89.42(16) . 3_655 ?
O11 Mo3 O19 166.66(16) . 3_655 ?
O13 Mo3 O19 79.05(17) . 3_655 ?
O9 Mo3 O19 80.19(13) . 3_655 ?
O12 Mo3 O18 166.15(16) . 3_655 ?
O11 Mo3 O18 87.71(16) . 3_655 ?
O13 Mo3 O18 84.12(16) . 3_655 ?
O9 Mo3 O18 72.29(13) . 3_655 ?
O19 Mo3 O18 78.98(11) 3_655 3_655 ?
O14 Mo4 O6 105.38(16) . . ?
O14 Mo4 O10 104.61(15) . . ?
O6 Mo4 O10 98.31(15) . . ?
O14 Mo4 O16 93.14(15) . . ?
O6 Mo4 O16 88.31(15) . . ?
O10 Mo4 O16 158.51(14) . . ?
O14 Mo4 O17 92.59(14) . . ?
O6 Mo4 O17 158.65(13) . . ?
O10 Mo4 O17 87.95(13) . . ?
O16 Mo4 O17 79.11(14) . . ?
O14 Mo4 O15 160.59(15) . . ?
O6 Mo4 O15 87.50(15) . . ?
O10 Mo4 O15 87.39(13) . . ?
O16 Mo4 O15 72.43(13) . . ?
O17 Mo4 O15 72.34(14) . . ?
O20 Mo5 O19 105.45(15) . . ?
O20 Mo5 O19 105.45(15) . 3_655 ?
O19 Mo5 O19 99.0(2) . 3_655 ?
O20 Mo5 O17 92.66(16) . 3_655 ?
O19 Mo5 O17 87.93(14) . 3_655 ?
O19 Mo5 O17 157.91(13) 3_655 3_655 ?
O20 Mo5 O17 92.66(16) . . ?
O19 Mo5 O17 157.91(13) . . ?
O19 Mo5 O17 87.93(14) 3_655 . ?
O17 Mo5 O17 78.53(17) 3_655 . ?
O20 Mo5 O15 160.0(2) . . ?
O19 Mo5 O15 87.28(12) . . ?
O19 Mo5 O15 87.29(12) 3_655 . ?
O17 Mo5 O15 72.04(11) 3_655 . ?
O17 Mo5 O15 72.04(11) . . ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
H1C N1 H1F 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
H2C N2 H2F 109.5 . . ?
H2D N2 H2F 109.5 . . ?
H2E N2 H2F 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
H3A N3 H3D 109.5 . . ?
H3B N3 H3D 109.4 . . ?
H3C N3 H3D 109.4 . . ?
H24A O24 H24B 107.4 . . ?
Mo1 O1 Mo1 120.7(2) . 3_655 ?
Mo1 O4 Mo2 167.52(19) . . ?
V1 O5 Mo1 127.23(13) . 3_655 ?
V1 O5 Mo1 127.23(13) . . ?
Mo1 O5 Mo1 93.31(16) 3_655 . ?
Mo4 O6 Mo1 144.22(17) . . ?
Mo2 O9 Mo3 119.33(17) . . ?
Mo4 O10 Mo2 144.79(18) . . ?
Mo3 O13 Mo3 165.3(3) 3_655 . ?
V1 O15 Mo4 117.37(13) . 3_655 ?
V1 O15 Mo4 117.37(13) . . ?
Mo4 O15 Mo4 100.51(15) 3_655 . ?
V1 O15 Mo5 116.68(19) . . ?
Mo4 O15 Mo5 100.99(13) 3_655 . ?
Mo4 O15 Mo5 100.99(13) . . ?
C1 O16 Mo4 117.97(15) . 3_655 ?
C1 O16 Mo4 117.96(15) . . ?
Mo4 O16 Mo4 112.78(19) 3_655 . ?
C2 O17 Mo4 117.8(3) . . ?
C2 O17 Mo5 118.2(3) . . ?
Mo4 O17 Mo5 112.76(13) . . ?
V1 O18 Mo3 127.87(17) . 3_655 ?
V1 O18 Mo2 127.01(17) . 3_655 ?
Mo3 O18 Mo2 93.48(12) 3_655 3_655 ?
Mo5 O19 Mo3 144.04(19) . 3_655 ?
H21A O21 H21B 104.5 . . ?
H22A O22 H22B 104.5 . . ?
H23A O23 H23B 69.0 . . ?
H4D N4 H4E 109.5 . . ?
H4D N4 H4F 109.5 . . ?
H4E N4 H4F 109.5 . . ?
H4D N4 H4G 109.5 . . ?
H4E N4 H4G 109.5 . . ?
H4F N4 H4G 109.5 . . ?
H25A O25 H25B 93.5 . . ?
O5 V1 O18 110.13(13) . 3_655 ?
O5 V1 O18 110.13(13) . . ?
O18 V1 O18 110.1(2) 3_655 . ?
O5 V1 O15 109.1(2) . . ?
O18 V1 O15 108.66(13) 3_655 . ?
O18 V1 O15 108.66(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O16 1.444(7) . ?
C1 C3 1.530(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O17 1.457(5) . ?
C2 C3 1.524(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.512(8) . ?
C3 C2 1.524(6) 3_655 ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
Mo1 O2 1.714(4) . ?
Mo1 O3 1.723(4) . ?
Mo1 O4 1.904(3) . ?
Mo1 O1 1.930(2) . ?
Mo1 O6 2.228(3) . ?
Mo1 O5 2.306(3) . ?
Mo2 O8 1.712(4) . ?
Mo2 O7 1.720(4) . ?
Mo2 O4 1.911(3) . ?
Mo2 O9 1.936(3) . ?
Mo2 O10 2.197(3) . ?
Mo2 O18 2.313(3) 3_655 ?
Mo3 O12 1.701(4) . ?
Mo3 O11 1.710(4) . ?
Mo3 O13 1.9099(9) . ?
Mo3 O9 1.953(4) . ?
Mo3 O19 2.228(3) 3_655 ?
Mo3 O18 2.296(3) 3_655 ?
Mo4 O14 1.705(3) . ?
Mo4 O6 1.773(3) . ?
Mo4 O10 1.774(3) . ?
Mo4 O16 2.134(2) . ?
Mo4 O17 2.142(3) . ?
Mo4 O15 2.311(3) . ?
Mo5 O20 1.701(5) . ?
Mo5 O19 1.770(3) . ?
Mo5 O19 1.770(3) 3_655 ?
Mo5 O17 2.149(3) 3_655 ?
Mo5 O17 2.149(3) . ?
Mo5 O15 2.319(4) . ?
N1 H1C 0.8899 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.9101 . ?
N1 H1F 0.9101 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.9098 . ?
N2 H2F 0.9102 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8902 . ?
N3 H3C 0.8899 . ?
N3 H3D 0.9100 . ?
O24 H24A 0.8488 . ?
O24 H24B 0.8486 . ?
O1 Mo1 1.930(2) 3_655 ?
O5 V1 1.686(4) . ?
O5 Mo1 2.306(3) 3_655 ?
O13 Mo3 1.9099(9) 3_655 ?
O15 V1 1.793(4) . ?
O15 Mo4 2.311(3) 3_655 ?
O16 Mo4 2.134(2) 3_655 ?
O18 V1 1.686(3) . ?
O18 Mo3 2.295(3) 3_655 ?
O18 Mo2 2.313(3) 3_655 ?
O19 Mo3 2.228(3) 3_655 ?
O21 H21A 0.8499 . ?
O21 H21B 0.8499 . ?
O22 H22A 0.8501 . ?
O22 H22B 0.8502 . ?
O23 H23A 0.7243 . ?
O23 H23B 0.6773 . ?
N4 H4D 0.8900 . ?
N4 H4E 0.8900 . ?
N4 H4F 0.8901 . ?
N4 H4G 0.9100 . ?
O25 H25A 1.0002 . ?
O25 H25B 0.8502 . ?
V1 O18 1.686(3) 3_655 ?