#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:39:39 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228901 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/16/7231640.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_7231640
loop_
_publ_author_name
'Wang, Fu-Rong'
'Li, Zi-Yan'
'Wei, Dong-Hui'
'Niu, Yun-Yin'
'Hou, Hong-Wei'
'Wu, Ben-Lai'
_publ_section_title
;
 The conformational behavior of multivalent tris(imidazolium)cyclophanes
 in the hybrids with metal (pseudo)halides or polyoxometalates
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7184
_journal_paper_doi               10.1039/C8CE01372A
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '4(C30 H33 N6), 4(H Mo5 O17), 6.5(H4 O2)'
_chemical_formula_sum            'C120 H162 Mo20 N24 O81'
_chemical_formula_weight         5155.53
_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'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-20 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.3449(3)
_cell_length_b                   20.7592(6)
_cell_length_c                   17.6129(6)
_cell_measurement_reflns_used    3020
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6250
_cell_measurement_theta_min      4.2470
_cell_volume                     4148.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -95.00  -59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000 -180.0000 36

#__ type_ start__ end____ width___ exp.time_
  2 omega  -41.00   -6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000    0.0000 35

#__ type_ start__ end____ width___ exp.time_
  3 omega   -8.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  150.0000 39

#__ type_ start__ end____ width___ exp.time_
  4 omega -103.00  -71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -77.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
  5 omega   16.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -60.0000 91

#__ type_ start__ end____ width___ exp.time_
  6 omega    0.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega   73.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000   30.0000 31

#__ type_ start__ end____ width___ exp.time_
  8 omega    1.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
  9 omega  -25.00   23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000    0.0000 48

#__ type_ start__ end____ width___ exp.time_
 10 omega   29.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00   95.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 55

#__ type_ start__ end____ width___ exp.time_
 12 omega   56.00  113.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 57

#__ type_ start__ end____ width___ exp.time_
 13 omega   50.00   85.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
 14 omega  102.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -60.0000 60

#__ type_ start__ end____ width___ exp.time_
 15 omega  108.00  155.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 47

#__ type_ start__ end____ width___ exp.time_
 16 omega   41.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 68

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 49

#__ type_ start__ end____ width___ exp.time_
 18 omega   37.00   82.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 45

#__ type_ start__ end____ width___ exp.time_
 19 omega   45.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
 20 omega   53.00   84.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0586860500
_diffrn_orient_matrix_UB_12      0.0663339500
_diffrn_orient_matrix_UB_13      -0.0106122000
_diffrn_orient_matrix_UB_21      0.1221672000
_diffrn_orient_matrix_UB_22      -0.0323581000
_diffrn_orient_matrix_UB_23      -0.0005255000
_diffrn_orient_matrix_UB_31      -0.0080539000
_diffrn_orient_matrix_UB_32      -0.0078622000
_diffrn_orient_matrix_UB_33      -0.0868206000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7783
_diffrn_reflns_point_group_measured_fraction_full 0.746
_diffrn_reflns_point_group_measured_fraction_max 0.746
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         4.259
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.817
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_description       prism
_exptl_crystal_F_000             2538
_exptl_crystal_size_max          0.3038
_exptl_crystal_size_mid          0.0916
_exptl_crystal_size_min          0.0304
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.056(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0547P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.441
_reflns_Friedel_fraction_full    0.474
_reflns_Friedel_fraction_max     0.474
_reflns_number_gt                2722
_reflns_number_total             2926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01372a2.cif
_cod_data_source_block           nyy2018061902
_cod_depositor_comments
'Adding full bibliography for 7231632--7231641.cif.'
_cod_database_code               7231640
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C30H37O19N6Mo5
_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.
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H17A(0.5) H17B(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) H12A(0.5) H13C(0.5) H13D(0.5) O14(0.125) H14A(0.125) H14B(0.125)
 H15A(0.5) H15B(0.5)
4.a Riding coordinates:
 C9(H9A,H9B), O12(H12A,H12B), O13(H13C,H13D), O14(H14A,H14B), O15(H15A,H15B),
 O15(H11A)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C13(H13A,H13B), C17(H17A,H17B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C11(H11), C12(H12), C15(H15), C20(H20)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_olex2_date_sample_data_collection 2018-06-22
_olex2_submission_special_instructions 'No special instructions were received'
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 0.7347(6) 0.4340(11) 0.038(3) Uani 1 2 d S T P . .
H1 H 0.5000 0.7699 0.4014 0.046 Uiso 1 2 calc RS T P . .
C2 C 0.5000 0.7363(6) 0.5100(10) 0.041(4) Uani 1 2 d S T P . .
H2 H 0.5000 0.7729 0.5404 0.050 Uiso 1 2 calc RS T P . .
C3 C 0.5000 0.6355(6) 0.4746(9) 0.034(3) Uani 1 2 d S T P . .
H3 H 0.5000 0.5907 0.4754 0.040 Uiso 1 2 calc RS T P . .
C4 C 0.5000 0.6546(8) 0.6167(11) 0.066(6) Uani 1 2 d S T P . .
H4A H 0.4308 0.6721 0.6415 0.080 Uiso 0.5 1 calc R . . . .
H4B H 0.5692 0.6721 0.6415 0.080 Uiso 0.5 1 calc R . . . .
C5 C 0.5000 0.5811(8) 0.6243(9) 0.050(5) Uani 1 2 d S T P . .
C6 C 0.3914(12) 0.5484(6) 0.6288(6) 0.042(3) Uani 1 1 d . . . . .
C7 C 0.3950(10) 0.4813(5) 0.6285(6) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.5000 0.4464(7) 0.6286(8) 0.035(3) Uani 1 2 d S T P . .
C9 C 0.2789(10) 0.4442(5) 0.6213(6) 0.039(3) Uani 1 1 d . . . . .
H9A H 0.2718 0.4055 0.6417 0.047 Uiso 1 1 d R . . . .
H9B H 0.2509 0.4710 0.6599 0.047 Uiso 1 1 d R . . . .
C10 C 0.2511(12) 0.3563(6) 0.5216(8) 0.051(3) Uani 1 1 d . . . . .
H10 H 0.2424 0.3210 0.5536 0.061 Uiso 1 1 calc R . . . .
C11 C 0.2496(11) 0.3539(5) 0.4452(8) 0.051(3) Uani 1 1 d . . . . .
H11 H 0.2396 0.3178 0.4147 0.062 Uiso 1 1 calc R . . . .
C12 C 0.2750(9) 0.4540(5) 0.4827(6) 0.034(2) Uani 1 1 d . . . . .
H12 H 0.2849 0.4985 0.4819 0.041 Uiso 1 1 calc R . . . .
C13 C 0.2793(9) 0.4387(5) 0.3427(6) 0.032(2) Uani 1 1 d . . . . .
H13A H 0.2133 0.4660 0.3289 0.039 Uiso 1 1 calc R . . . .
H13B H 0.2795 0.4016 0.3092 0.039 Uiso 1 1 calc R . . . .
C14 C 0.3947(9) 0.4761(5) 0.3338(6) 0.030(2) Uani 1 1 d . . . . .
C15 C 0.3950(9) 0.5425(5) 0.3295(6) 0.031(2) Uani 1 1 d . . . . .
H15 H 0.3239 0.5646 0.3262 0.037 Uiso 1 1 calc R . . . .
C16 C 0.5000 0.5766(7) 0.3300(8) 0.032(3) Uani 1 2 d S T P . .
C17 C 0.5000 0.6496(7) 0.3342(9) 0.035(3) Uani 1 2 d S T P . .
H17A H 0.5692 0.6662 0.3085 0.042 Uiso 0.5 1 calc R . . . .
H17B H 0.4308 0.6662 0.3085 0.042 Uiso 0.5 1 calc R . . . .
C18 C 0.2763(15) 0.5866(7) 0.6325(9) 0.067(4) Uani 1 1 d . . . . .
H18A H 0.2709 0.6082 0.6806 0.100 Uiso 1 1 calc GR . . . .
H18B H 0.2107 0.5577 0.6268 0.100 Uiso 1 1 calc GR . . . .
H18C H 0.2749 0.6179 0.5923 0.100 Uiso 1 1 calc GR . . . .
C19 C 0.5000 0.3736(8) 0.6273(11) 0.051(5) Uani 1 2 d S T P . .
H19A H 0.5273 0.3588 0.5788 0.077 Uiso 0.5 1 calc GR . . A -1
H19B H 0.4214 0.3581 0.6360 0.077 Uiso 0.5 1 calc GR . . A -1
H19C H 0.5512 0.3577 0.6664 0.077 Uiso 0.5 1 calc GR . . A -1
C20 C 0.5000 0.4420(6) 0.3365(8) 0.026(3) Uani 1 2 d S T P . .
H20 H 0.5000 0.3973 0.3399 0.031 Uiso 1 2 calc RS T P . .
N1 N 0.5000 0.6716(5) 0.4139(7) 0.029(3) Uani 1 2 d S T P . .
N2 N 0.5000 0.6736(5) 0.5344(7) 0.033(3) Uani 1 2 d S T P . .
N3 N 0.2674(8) 0.4187(4) 0.5450(5) 0.034(2) Uani 1 1 d . . . . .
N4 N 0.2664(7) 0.4172(4) 0.4222(5) 0.0290(19) Uani 1 1 d . . . . .
Mo1 Mo 0.85151(6) 0.72335(3) 0.27054(4) 0.02577(19) Uani 1 1 d . . . . .
Mo2 Mo 0.85227(6) 0.66077(3) 0.43438(5) 0.0277(2) Uani 1 1 d . . . . .
Mo3 Mo 1.0000 0.57288(5) 0.28384(9) 0.0408(4) Uani 1 2 d S T P . .
O1 O 0.8621(6) 0.8053(3) 0.2694(5) 0.0370(16) Uani 1 1 d . . . . .
O2 O 0.7533(7) 0.7053(4) 0.2019(5) 0.047(2) Uani 1 1 d . . . . .
O3 O 1.0000 0.7022(5) 0.2237(6) 0.031(2) Uani 1 2 d S T P . .
O4 O 0.7671(6) 0.7146(3) 0.3654(4) 0.0308(16) Uani 1 1 d . . . . .
O5 O 0.8547(7) 0.7103(4) 0.5118(5) 0.043(2) Uani 1 1 d . . . . .
O6 O 0.7536(6) 0.6006(3) 0.4564(4) 0.0387(18) Uani 1 1 d . . . . .
O7 O 1.0000 0.6154(5) 0.4445(7) 0.036(2) Uani 1 2 d S T P . .
O8 O 0.8706(6) 0.6198(3) 0.3106(4) 0.0311(16) Uani 1 1 d . . . . .
O9 O 1.0000 0.5563(8) 0.1891(9) 0.073(5) Uani 1 2 d S T P . .
O10 O 1.0000 0.5006(6) 0.3328(10) 0.072(5) Uani 1 2 d S T P . .
O11 O 1.0000 0.7229(4) 0.3721(6) 0.027(2) Uani 1 2 d S T P . .
O12 O 1.0000 0.3556(8) 0.3129(12) 0.109(7) Uani 1 2 d S T P . .
H12A H 0.9536 0.3495 0.2756 0.164 Uiso 0.5 1 d R . . . .
H12B H 1.0000 0.3956 0.3204 0.164 Uiso 1 2 d RS T P . .
O13 O 0.0000 0.4854(13) 0.5163(17) 0.159(10) Uani 1 2 d S TU P . .
H13C H 0.0330 0.4972 0.5663 0.238 Uiso 0.5 1 d R . . . .
H13D H -0.0288 0.5246 0.5063 0.238 Uiso 0.5 1 d R . . . .
O14 O 1.0000 0.374(3) 0.587(4) 0.09(2) Uani 0.25 2 d S TU P . .
H14A H 1.0456 0.3941 0.5567 0.140 Uiso 0.125 1 d R . . . .
H14B H 0.9343 0.3662 0.5657 0.140 Uiso 0.125 1 d R . . . .
O15 O 0.5000 0.1984(15) 0.6622(14) 0.162(11) Uani 1 2 d S T P . .
H15A H 0.4524 0.2043 0.7034 0.243 Uiso 0.5 1 d R . . . .
H15B H 0.4564 0.2173 0.6305 0.243 Uiso 0.5 1 d R . . . .
H11A H 1.0000 0.7596 0.3994 0.243 Uiso 1 2 d RS T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 13 0 0.0278 0.0712 13.4712 0.1472 0.8962 -0.4273 -0.1193
0 -13 0 0.0010 -0.0665 -13.4723 -0.0218 -0.8973 0.4278 0.1083
-1 -1 -11 0.1351 -0.8332 -1.4254 -11.2942 -0.0236 -0.0497 0.9985
7 0 0 0.0490 7.3650 -0.0540 -0.1151 0.4299 0.9016 -0.0489
0 1 11 0.1525 0.1260 1.4383 11.3663 -0.0178 -0.0371 -0.9992
-7 0 -1 0.0340 -7.3571 -0.0273 -0.5270 -0.4280 -0.8976 0.1052
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
C2 C1 H1 126.7 . .
C2 C1 N1 106.6(14) . .
N1 C1 H1 126.7 . .
C1 C2 H2 126.6 . .
C1 C2 N2 106.9(13) . .
N2 C2 H2 126.6 . .
N1 C3 H3 126.0 . .
N1 C3 N2 108.0(12) . .
N2 C3 H3 126.0 . .
H4A C4 H4B 108.1 . .
C5 C4 H4A 109.6 . .
C5 C4 H4B 109.6 . .
N2 C4 H4A 109.6 . .
N2 C4 H4B 109.6 . .
N2 C4 C5 110.3(14) . .
C6 C5 C4 119.1(8) . .
C6 C5 C4 119.1(8) 3_655 .
C6 C5 C6 121.9(15) . 3_655
C5 C6 C18 119.9(12) . .
C7 C6 C5 117.2(12) . .
C7 C6 C18 122.9(12) . .
C6 C7 C8 123.0(12) . .
C6 C7 C9 118.6(10) . .
C8 C7 C9 118.2(10) . .
C7 C8 C7 117.4(15) 3_655 .
C7 C8 C19 121.3(7) . .
C7 C8 C19 121.3(7) 3_655 .
C7 C9 H9A 120.2 . .
C7 C9 H9B 86.1 . .
H9A C9 H9B 102.5 . .
N3 C9 C7 109.8(9) . .
N3 C9 H9A 92.0 . .
N3 C9 H9B 149.4 . .
C11 C10 H10 125.1 . .
C11 C10 N3 109.8(10) . .
N3 C10 H10 125.1 . .
C10 C11 H11 127.6 . .
C10 C11 N4 104.8(10) . .
N4 C11 H11 127.6 . .
N3 C12 H12 124.9 . .
N4 C12 H12 124.9 . .
N4 C12 N3 110.2(9) . .
H13A C13 H13B 108.2 . .
C14 C13 H13A 109.7 . .
C14 C13 H13B 109.7 . .
N4 C13 H13A 109.7 . .
N4 C13 H13B 109.7 . .
N4 C13 C14 109.6(8) . .
C15 C14 C13 120.9(10) . .
C15 C14 C20 120.5(10) . .
C20 C14 C13 118.3(9) . .
C14 C15 H15 119.6 . .
C14 C15 C16 120.8(10) . .
C16 C15 H15 119.6 . .
C15 C16 C15 118.6(14) . 3_655
C15 C16 C17 120.7(7) 3_655 .
C15 C16 C17 120.7(7) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 108.1 . .
N1 C17 C16 110.9(12) . .
N1 C17 H17A 109.5 . .
N1 C17 H17B 109.5 . .
C6 C18 H18A 109.5 . .
C6 C18 H18B 109.5 . .
C6 C18 H18C 109.5 . .
H18A C18 H18B 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C8 C19 H19A 109.5 . .
C8 C19 H19B 109.5 . .
C8 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C14 C20 C14 118.7(13) 3_655 .
C14 C20 H20 120.6 . .
C14 C20 H20 120.6 3_655 .
C1 N1 C17 123.2(12) . .
C3 N1 C1 109.9(13) . .
C3 N1 C17 126.9(12) . .
C2 N2 C4 123.6(13) . .
C3 N2 C2 108.6(13) . .
C3 N2 C4 127.9(13) . .
C10 N3 C9 129.5(10) . .
C12 N3 C9 124.0(9) . .
C12 N3 C10 106.4(10) . .
C11 N4 C13 125.2(9) . .
C12 N4 C11 108.8(9) . .
C12 N4 C13 125.9(8) . .
O1 Mo1 Mo2 114.8(3) . .
O1 Mo1 O3 99.3(4) . .
O1 Mo1 O4 97.9(3) . .
O1 Mo1 O8 160.1(3) . .
O1 Mo1 O11 88.0(3) . .
O2 Mo1 Mo2 124.3(3) . .
O2 Mo1 O1 105.1(4) . .
O2 Mo1 O3 102.7(4) . .
O2 Mo1 O4 105.7(4) . .
O2 Mo1 O8 94.3(3) . .
O2 Mo1 O11 166.9(4) . .
O3 Mo1 Mo2 107.1(3) . .
O3 Mo1 O4 141.4(4) . .
O3 Mo1 O8 80.5(3) . .
O3 Mo1 O11 73.2(3) . .
O4 Mo1 Mo2 34.5(2) . .
O4 Mo1 O8 72.0(3) . .
O4 Mo1 O11 73.2(3) . .
O8 Mo1 Mo2 47.79(18) . .
O8 Mo1 O11 72.8(3) . .
O11 Mo1 Mo2 48.13(17) . .
O4 Mo2 Mo1 34.9(2) . .
O4 Mo2 O7 141.5(4) . .
O4 Mo2 O8 70.5(3) . .
O4 Mo2 O11 75.3(3) . .
O5 Mo2 Mo1 118.7(3) . .
O5 Mo2 O4 99.4(4) . .
O5 Mo2 O6 105.5(4) . .
O5 Mo2 O7 101.9(4) . .
O5 Mo2 O8 163.2(3) . .
O5 Mo2 O11 91.7(4) . .
O6 Mo2 Mo1 120.1(3) . .
O6 Mo2 O4 103.8(3) . .
O6 Mo2 O7 100.9(3) . .
O6 Mo2 O8 90.2(3) . .
O6 Mo2 O11 162.5(3) . .
O7 Mo2 Mo1 106.7(3) . .
O7 Mo2 O8 80.4(4) . .
O7 Mo2 O11 72.3(3) . .
O8 Mo2 Mo1 45.78(16) . .
O8 Mo2 O11 72.9(3) . .
O11 Mo2 Mo1 50.21(19) . .
O8 Mo3 O8 107.2(4) 3_755 .
O9 Mo3 O8 111.2(4) . .
O9 Mo3 O8 111.2(4) . 3_755
O9 Mo3 O10 108.2(8) . .
O10 Mo3 O8 109.5(4) . 3_755
O10 Mo3 O8 109.5(4) . .
Mo1 O3 Mo1 121.9(5) . 3_755
Mo2 O4 Mo1 110.7(3) . .
Mo2 O7 Mo2 120.5(5) 3_755 .
Mo1 O8 Mo2 86.4(2) . .
Mo3 O8 Mo1 120.1(3) . .
Mo3 O8 Mo2 120.3(4) . .
Mo1 O11 Mo1 86.5(3) . 3_755
Mo1 O11 H11A 112.6 . .
Mo1 O11 H11A 112.6 3_755 .
Mo2 O11 Mo1 81.66(12) 3_755 3_755
Mo2 O11 Mo1 145.0(4) . 3_755
Mo2 O11 Mo1 145.0(4) 3_755 .
Mo2 O11 Mo1 81.66(12) . .
Mo2 O11 Mo2 89.4(3) . 3_755
Mo2 O11 H11A 102.3 . .
Mo2 O11 H11A 102.3 3_755 .
H12A O12 H12B 105.5 . .
H13C O13 H13D 95.1 . .
H14A O14 H14B 110.7 . .
H15A O15 H15B 96.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 H1 0.9300 .
C1 C2 1.34(2) .
C1 N1 1.356(17) .
C2 H2 0.9300 .
C2 N2 1.371(18) .
C3 H3 0.9300 .
C3 N1 1.306(18) .
C3 N2 1.318(19) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.53(2) .
C4 N2 1.50(2) .
C5 C6 1.409(15) .
C5 C6 1.409(15) 3_655
C6 C7 1.392(15) .
C6 C18 1.530(17) .
C7 C8 1.394(13) .
C7 C9 1.532(15) .
C8 C7 1.394(13) 3_655
C8 C19 1.51(2) .
C9 H9A 0.8845 .
C9 H9B 0.9338 .
C9 N3 1.450(14) .
C10 H10 0.9300 .
C10 C11 1.345(18) .
C10 N3 1.371(14) .
C11 H11 0.9300 .
C11 N4 1.388(13) .
C12 H12 0.9300 .
C12 N3 1.323(13) .
C12 N4 1.316(13) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C14 1.530(13) .
C13 N4 1.476(13) .
C14 C15 1.381(14) .
C14 C20 1.388(12) .
C15 H15 0.9300 .
C15 C16 1.386(13) .
C16 C15 1.386(13) 3_655
C16 C17 1.517(19) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C17 N1 1.477(19) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 C14 1.388(12) 3_655
C20 H20 0.9300 .
Mo1 Mo2 3.1646(11) .
Mo1 O1 1.706(6) .
Mo1 O2 1.686(8) .
Mo1 O3 1.927(5) .
Mo1 O4 1.934(7) .
Mo1 O8 2.272(7) .
Mo1 O11 2.458(7) .
Mo2 O4 1.913(7) .
Mo2 O5 1.708(8) .
Mo2 O6 1.722(7) .
Mo2 O7 1.931(5) .
Mo2 O8 2.349(7) .
Mo2 O11 2.382(7) .
Mo3 O8 1.825(6) 3_755
Mo3 O8 1.825(6) .
Mo3 O9 1.704(15) .
Mo3 O10 1.731(15) .
O3 Mo1 1.927(5) 3_755
O7 Mo2 1.930(5) 3_755
O11 Mo1 2.458(7) 3_755
O11 Mo2 2.382(7) 3_755
O11 H11A 0.9009 .
O12 H12A 0.8507 .
O12 H12B 0.8418 .
O13 H13C 0.9875 .
O13 H13D 0.8946 .
O14 H14A 0.8494 .
O14 H14B 0.8496 .
O15 H15A 0.9137 .
O15 H15B 0.8431 .
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
O12 H12A O15 0.85 2.29 2.88(3) 126.4 6_654
O12 H12B O10 0.84 2.19 3.03(2) 176.7 .
O13 H13C O9 0.99 2.46 3.16(3) 128.0 2_665
O13 H13D O7 0.89 2.20 2.98(3) 145.3 1_455
O14 H14A N3 0.85 2.58 3.26(3) 137.9 1_655
O14 H14A O13 0.85 2.09 2.62(8) 120.4 1_655
O14 H14B N3 0.85 2.56 3.26(3) 139.9 3_655
O15 H15A O2 0.91 2.99 3.57(2) 122.6 2_665
O15 H15B O5 0.84 2.39 3.13(2) 146.4 5_445
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 C2 N2 C3 0.000(6) . .
C1 C2 N2 C4 180.000(7) . .
C2 C1 N1 C3 0.000(6) . .
C2 C1 N1 C17 180.000(6) . .
C4 C5 C6 C7 174.1(13) . .
C4 C5 C6 C18 -5(2) . .
C5 C4 N2 C2 180.000(6) . .
C5 C4 N2 C3 0.000(7) . .
C5 C6 C7 C8 3.9(18) . .
C5 C6 C7 C9 -171.0(11) . .
C6 C5 C6 C7 -8(2) 3_655 .
C6 C5 C6 C18 173.3(10) 3_655 .
C6 C7 C8 C7 0(2) . 3_655
C6 C7 C8 C19 -179.3(13) . .
C6 C7 C9 N3 104.3(11) . .
C7 C9 N3 C10 123.5(12) . .
C7 C9 N3 C12 -54.2(14) . .
C8 C7 C9 N3 -70.8(13) . .
C9 C7 C8 C7 174.6(8) . 3_655
C9 C7 C8 C19 -4.4(19) . .
C10 C11 N4 C12 -1.0(14) . .
C10 C11 N4 C13 175.7(10) . .
C11 C10 N3 C9 -177.6(11) . .
C11 C10 N3 C12 0.4(14) . .
C13 C14 C15 C16 172.7(10) . .
C13 C14 C20 C14 -175.5(8) . 3_655
C14 C13 N4 C11 -124.3(11) . .
C14 C13 N4 C12 51.9(13) . .
C14 C15 C16 C15 4(2) . 3_655
C14 C15 C16 C17 -173.1(12) . .
C15 C14 C20 C14 -1(2) . 3_655
C15 C16 C17 N1 -88.8(12) 3_655 .
C15 C16 C17 N1 88.8(12) . .
C16 C17 N1 C1 180.000(6) . .
C16 C17 N1 C3 0.000(6) . .
C18 C6 C7 C8 -177.1(12) . .
C18 C6 C7 C9 8.0(16) . .
C20 C14 C15 C16 -1.9(18) . .
N1 C1 C2 N2 0.000(6) . .
N1 C3 N2 C2 0.000(6) . .
N1 C3 N2 C4 180.000(7) . .
N2 C3 N1 C1 0.000(6) . .
N2 C3 N1 C17 180.000(6) . .
N2 C4 C5 C6 90.8(13) . 3_655
N2 C4 C5 C6 -90.8(13) . .
N3 C10 C11 N4 0.3(15) . .
N3 C12 N4 C11 1.3(13) . .
N3 C12 N4 C13 -175.4(9) . .
N4 C12 N3 C9 177.1(9) . .
N4 C12 N3 C10 -1.1(13) . .
N4 C13 C14 C15 -103.0(11) . .
N4 C13 C14 C20 71.8(12) . .
O8 Mo3 O8 Mo1 53.1(6) 3_755 .
O8 Mo3 O8 Mo2 -51.7(6) 3_755 .
O9 Mo3 O8 Mo1 -68.6(7) . .
O9 Mo3 O8 Mo2 -173.4(6) . .
O10 Mo3 O8 Mo1 171.8(6) . .
O10 Mo3 O8 Mo2 67.1(6) . .
