#------------------------------------------------------------------------------
#$Date: 2021-10-06 17:51:35 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269676 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/32/7243291.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_7243291
loop_
_publ_author_name
'Bebić, Nikol'
'Topić, Edi'
'Mandarić, Mirna'
'Hrenar, Tomica'
'Vrdoljak, Višnja'
_publ_section_title
;
 Extending the structural landscape of Mo(vi) hydrazonato
 inorganic--organic POM-hybrids: an experimental and computational study
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              6349
_journal_page_last               6358
_journal_paper_doi               10.1039/D1CE00861G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'Mo8 O26, 2(C14 H15 Mo N3 O6), 4(H2 O), 1.5(C4 H6 N2)'
_chemical_formula_sum            'C34 H47 Mo10 N9 O42'
_chemical_formula_weight         2213.20
_chemical_name_systematic
'[N-(2-oxo-4-methoxybenzylidene)isonicotinoylhydrazonato](aqua)dioxomolybdenum(vi) octamolybdate acetonitrile solvate hydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                100.3730(10)
_cell_angle_beta                 104.041(2)
_cell_angle_gamma                106.410(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2611(2)
_cell_length_b                   10.5249(2)
_cell_length_c                   15.9967(2)
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.6620
_cell_measurement_theta_min      4.5340
_cell_volume                     1549.28(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     91.00 130.00   0.50    0.25    --  113.25  77.00 120.00   78
  2  ω    133.00 178.00   0.50    0.25    --  113.25  77.00 120.00   90
  3  ω     93.00 172.00   0.50    0.25    --  113.25  77.00 150.00  158
  4  ω    100.00 175.00   0.50    0.25    --  113.25  77.00  60.00  150
  5  ω     94.00 155.00   0.50    0.25    --  113.25  77.00  30.00  122
  6  ω    148.00 178.00   0.50    0.25    --  113.25  77.00 -90.00   60
  7  ω    136.00 177.00   0.50    0.25    --  113.25  77.00-120.00   82
  8  ω     91.00 136.00   0.50    0.25    --  113.25  77.00-180.00   90
  9  ω     91.00 130.00   0.50    0.25    --  113.25  77.00-120.00   78
 10  ω     94.00 139.00   0.50    0.25    --  113.25  77.00 -90.00   90
 11  ω    104.00 175.00   0.50    0.25    --  113.25  77.00-150.00  142
 12  ω    100.00 135.00   0.50    0.25    --  113.25  61.00 -30.00   70
 13  ω     91.00 173.00   0.50    0.25    --  113.25  77.00  90.00  164
 14  ω     94.00 169.00   0.50    0.25    --  113.25  77.00 -30.00  150
 15  ω    102.00 149.00   0.50    0.25    --  113.25  61.00  90.00   94
 16  ω     91.00 156.00   0.50    0.25    --  113.25  77.00 -60.00  130
 17  ω    115.00 177.00   0.50    0.25    --  113.25  61.00 -60.00  124
 18  ω    100.00 162.00   0.50    0.25    --  113.25  61.00 -90.00  124
 19  ω     98.00 171.00   0.50    0.25    --  113.25  61.00-120.00  146
 20  ω     99.00 176.00   0.50    0.25    --  113.25  61.00-180.00  154
 21  ω     97.00 150.00   0.50    0.25    --  113.25  61.00-150.00  106
 22  ω    108.00 155.00   0.50    0.25    --  113.25  61.00   0.00   94
 23  ω    127.00 167.00   0.50    0.25    --  113.25  30.00  30.00   80
 24  ω    100.00 156.00   0.50    0.25    --  113.25  61.00  60.00  112
 25  ω    107.00 176.00   0.50    0.25    --  113.25  51.00 131.00  138
 26  ω     99.00 125.00   0.50    0.25    --  113.25  61.00 150.00   52
 27  ω     34.00  67.00   0.50    0.06    --   48.02  51.00 131.00   66
 28  ω   -120.00 -79.00   0.50    0.06    --  -48.02 -77.00  30.00   82
 29  ω    -57.00 -25.00   0.50    0.06    --  -48.02 -77.00 -90.00   64
 30  ω    -54.00 -25.00   0.50    0.06    --  -48.02 -77.00 -30.00   58
 31  ω    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00-150.00   62
 32  ω    -95.00 -25.00   0.50    0.06    --  -48.02 -77.00-180.00  140
 33  ω   -113.00 -87.00   0.50    0.06    --  -48.02 -77.00-150.00   52
 34  ω   -108.00 -82.00   0.50    0.06    --  -48.02 -77.00 -90.00   52
 35  ω    -61.00 -33.00   0.50    0.06    --  -48.02 -57.00 -60.00   56
 36  ω    -64.00 -26.00   0.50    0.06    --  -48.02 -77.00  30.00   76
 37  ω    -53.00 -25.00   0.50    0.06    --  -48.02 -77.00  90.00   56
 38  ω    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00 120.00   62
 39  ω    -89.00 -63.00   0.50    0.06    --  -48.02 -77.00 120.00   52
 40  ω    -80.00 -34.00   0.50    0.06    --  -48.02 -51.00 -14.00   92
 41  ω    -92.00 -36.00   0.50    0.06    --  -48.02 -38.00  30.00  112
 42  ω   -119.00 -37.00   0.50    0.06    --  -48.02 -38.00  90.00  164
 43  ω   -119.00 -93.00   0.50    0.06    --  -48.02 -51.00 -14.00   52
 44  ω   -118.00 -68.00   0.50    0.06    --  -48.02 -57.00 -60.00  100
 45  ω    -64.00 -37.00   0.50    0.06    --  -48.02 -38.00-120.00   54
 46  ω    -60.00 -35.00   0.50    0.06    --  -48.02 -57.00-150.00   50
 47  ω   -121.00 -75.00   0.50    0.06    --  -48.02 -19.00-180.00   92
 48  ω    -71.00 -44.00   0.50    0.06    --  -48.02 -19.00-180.00   54
 49  ω    -57.00 -19.00   0.50    0.25    --  -91.75  61.00 -60.00   76
 50  ω    -44.00  23.00   0.50    0.06    --  -48.02  51.00 131.00  134
 51  ω    -52.00 -27.00   0.50    0.25    --  -91.75  51.00 131.00   50
 52  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  60.00   52
 53  ω   -139.00-113.00   0.50    0.25    --  -91.75 -77.00 -60.00   52
 54  ω   -105.00 -70.00   0.50    0.25    --  -91.75 -77.00 -30.00   70
 55  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -60.00   50
 56  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -90.00   50
 57  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00-120.00   50
 58  ω   -122.00 -69.00   0.50    0.25    --  -91.75 -77.00-180.00  106
 59  ω   -163.00-129.00   0.50    0.25    --  -91.75 -77.00-180.00   68
 60  ω   -154.00-128.00   0.50    0.25    --  -91.75 -77.00   0.00   52
 61  ω    -97.00 -71.00   0.50    0.25    --  -91.75 -77.00  30.00   52
 62  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00   0.00   50
 63  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  94.40   52
 64  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00 150.00   52
 65  ω   -103.00 -69.00   0.50    0.25    --  -91.75 -76.00 123.13   68
 66  ω   -147.00-121.00   0.50    0.25    --  -91.75 -76.00 123.13   52
 67  ω   -107.00 -69.00   0.50    0.25    --  -91.75 -76.00  50.46   76
 68  ω   -100.00 -70.00   0.50    0.25    --  -91.75 -75.00 132.77   60
 69  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -75.00  33.55   50
 70  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  10.45   50
 71  ω   -103.00 -70.00   0.50    0.25    --  -91.75 -75.00 -17.78   66
 72  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-108.94   50
 73  ω    -96.00 -70.00   0.50    0.25    --  -91.75 -75.00-142.63   52
 74  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-174.72   50
 75  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-160.09   50
 76  ω    -96.00 -70.00   0.50    0.25    --  -91.75 -74.00 -73.47   52
 77  ω   -107.00 -71.00   0.50    0.25    --  -91.75 -71.00 -52.45   72
 78  ω    -99.00 -74.00   0.50    0.25    --  -91.75 -63.00-148.79   50
 79  ω   -154.00-128.00   0.50    0.25    --  -91.75 -74.00-108.94   52
 80  ω   -145.00-120.00   0.50    0.25    --  -91.75 -51.00 -14.00   50
 81  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  73.92   50
 82  ω    -98.00 -71.00   0.50    0.25    --  -91.75 -71.00 101.08   54
 83  ω    -99.00 -74.00   0.50    0.25    --  -91.75 -68.00 158.24   50
 84  ω    104.00 165.00   0.50    0.25    --  113.25 125.00   0.00  122
 85  ω    123.00 148.00   0.50    0.25    --  113.25 125.00 -30.00   50
 86  ω     43.00  68.00   0.50    0.25    --  113.25 -61.00  90.00   50
 87  ω     42.00  69.00   0.50    0.25    --  113.25 -61.00  30.00   54
 88  ω     47.00  89.00   0.50    0.25    --  113.25 -77.00 -60.00   84
 89  ω     43.00  96.00   0.50    0.25    --  113.25 -77.00 -90.00  106
 90  ω    -23.00  53.00   0.50    0.06    --   48.02 -51.00 -14.00  152
 91  ω     43.00  97.00   0.50    0.25    --  113.25 -95.00  90.00  108
 92  ω     71.00 117.00   0.50    0.25    --  113.25-132.00 172.24   92
 93  ω     85.00 111.00   0.50    0.25    --  113.25-125.00  90.00   52
 94  ω     42.00  81.00   0.50    0.25    --  113.25-125.00  90.00   78
 95  ω     76.00 111.00   0.50    0.25    --  113.25-125.00   0.00   70
 96  ω     45.00  71.00   0.50    0.25    --  113.25-125.00   0.00   52
 97  ω     43.00 111.00   0.50    0.25    --  113.25-125.00 -90.00  136
 98  ω     43.00 111.00   0.50    0.25    --  113.25-125.00-120.00  136
 99  ω     44.00 107.00   0.50    0.25    --  113.25-125.00-150.00  126
100  ω     36.00  78.00   0.50    0.06    --   48.02-125.00-150.00   84
101  ω     46.00 111.00   0.50    0.25    --  113.25-125.00 -60.00  130
102  ω     78.00 108.00   0.50    0.25    --  113.25-112.00  43.18   60
103  ω     47.00 102.00   0.50    0.25    --  113.25-125.00  30.00  110
104  ω     45.00  75.00   0.50    0.25    --  113.25-112.00  43.18   60
105  ω     81.00 106.00   0.50    0.25    --  113.25-102.00  36.80   50
106  ω     86.00 111.00   0.50    0.25    --  113.25-125.00 120.00   50
107  ω     44.00  69.00   0.50    0.25    --  113.25-125.00 120.00   50
108  ω     64.00  90.00   0.50    0.25    --  113.25 -95.00 150.00   52
109  ω     51.00  76.00   0.50    0.25    --  113.25-102.00  36.80   50
110  ω      6.00  82.00   0.50    0.06    --   48.02 -99.00-180.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.744
_diffrn_reflns_theta_min         4.545
_exptl_absorpt_coefficient_mu    17.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00072(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_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)+(0.0473P)²+5.7164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6244
_reflns_number_total             6624
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_653
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_original_cell_volume        1549.28(5)
_cod_database_code               7243291
_shelx_shelxl_version_number     2018/3
_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_max   0.343
_shelx_estimated_absorpt_t_min   0.256
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3-N3
 0.86 with sigma of 0.02
 N4-C15
 1.14 with sigma of 0.02
 C16-N4
 2.593 with sigma of 0.02
 C15-N4
 1.137 with sigma of 0.01
 C15-C16
 1.456 with sigma of 0.01
 N4-C16
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C17) = Uanis(C18A)
Uanis(C15) = Uanis(C16)
Uanis(C17) = Uanis(C18)
Uanis(N5) = Uanis(C17)
4. Rigid body (RIGU) restrains
 N4, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C15(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C18A(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C18(0.5) H18D(0.5) H18E(0.5) H18F(0.5) O21(0.5)
 H21A(0.5) H21B(0.5) O21A(0.5) H21C(0.5) H21D(0.5)
6.a Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O21A(H21C,H21D)
6.b Rotating group:
 O5(H5A,H5B)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C13(H13), C10(H10), C7(H7), C11(H11), C6(H6), C12(H12), C3(H3A), C5(H5)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C18(H18D,H18E,
 H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_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_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
Mo3 Mo 0.49559(3) 0.89956(3) 0.39677(2) 0.01448(9) Uani 1 1 d . . . . .
Mo2 Mo 0.80419(3) 1.07158(3) 0.54314(2) 0.01556(9) Uani 1 1 d . . . . .
Mo4 Mo 0.39513(3) 0.74213(3) 0.53544(2) 0.01817(10) Uani 1 1 d . . . . .
Mo5 Mo 0.70569(3) 0.91165(3) 0.68670(2) 0.01876(10) Uani 1 1 d . . . . .
Mo1 Mo 0.66523(4) 0.44000(4) 0.17980(3) 0.02862(11) Uani 1 1 d . . . . .
O12 O 0.6651(3) 1.0633(3) 0.42886(18) 0.0159(5) Uani 1 1 d . . . . .
O14 O 0.5061(3) 0.7980(3) 0.6589(2) 0.0218(6) Uani 1 1 d . . . . .
O11 O 0.5780(3) 0.9260(3) 0.53804(18) 0.0146(5) Uani 1 1 d . . . . .
O15 O 0.8339(3) 1.0641(3) 0.66369(19) 0.0205(6) Uani 1 1 d . . . . .
O13 O 0.3269(3) 0.7941(3) 0.42285(18) 0.0157(5) Uani 1 1 d . . . . .
O17 O 0.4020(3) 0.9285(3) 0.29893(19) 0.0188(6) Uani 1 1 d . . . . .
O7 O 0.8501(3) 0.9353(3) 0.5008(2) 0.0225(6) Uani 1 1 d . . . . .
O8 O 0.5595(3) 0.7751(3) 0.3621(2) 0.0233(6) Uani 1 1 d . . . . .
O16 O 0.9444(3) 1.2138(3) 0.5542(2) 0.0247(6) Uani 1 1 d . . . . .
O9 O 0.4628(4) 0.6249(3) 0.4933(2) 0.0286(7) Uani 1 1 d . . . . .
O5 O 0.5331(4) 0.4395(4) 0.2826(2) 0.0334(8) Uani 1 1 d . . . . .
H5A H 0.509512 0.357390 0.296320 0.050 Uiso 1 1 d R U . . .
H5B H 0.587282 0.499479 0.336748 0.050 Uiso 1 1 d R U . . .
O2 O 0.7230(3) 0.6429(3) 0.2352(2) 0.0301(7) Uani 1 1 d . . . . .
O10 O 0.7636(3) 0.7856(3) 0.6425(2) 0.0281(7) Uani 1 1 d . . . . .
O18 O 0.2344(3) 0.6467(3) 0.5424(2) 0.0289(7) Uani 1 1 d . . . . .
O1 O 0.5199(4) 0.2613(4) 0.1224(2) 0.0365(8) Uani 1 1 d . . . . .
O19 O 0.7699(4) 0.9407(4) 0.7987(2) 0.0309(7) Uani 1 1 d . . . . .
O4 O 0.7756(4) 0.4031(4) 0.2634(3) 0.0430(10) Uani 1 1 d . . . . .
O20 O 0.7410(5) 0.6384(4) 0.4562(3) 0.0457(10) Uani 1 1 d G . . . .
H20A H 0.685935 0.642378 0.489498 0.069 Uiso 1 1 d G U . . .
H20B H 0.793116 0.723639 0.465009 0.069 Uiso 1 1 d G U . . .
O3 O 0.7485(4) 0.4539(4) 0.1012(3) 0.0432(9) Uani 1 1 d . . . . .
N1 N 0.4898(4) 0.5099(4) 0.1159(2) 0.0254(8) Uani 1 1 d . . . . .
N3 N 0.8156(4) 1.1410(4) 0.2923(3) 0.0296(8) Uani 1 1 d D . . . .
N2 N 0.5214(4) 0.6524(4) 0.1383(2) 0.0240(7) Uani 1 1 d . . . . .
H2 H 0.466207 0.695508 0.114472 0.029 Uiso 1 1 calc R U . . .
C13 C 0.6273(5) 0.9423(5) 0.1992(3) 0.0256(9) Uani 1 1 d . . . . .
H13 H 0.535803 0.900492 0.155403 0.031 Uiso 1 1 calc R U . . .
O6 O 0.1556(5) -0.1345(4) -0.0708(3) 0.0618(13) Uani 1 1 d . . . . .
C8 C 0.6438(5) 0.7107(5) 0.1991(3) 0.0238(9) Uani 1 1 d . . . . .
C10 C 0.8377(5) 0.9262(5) 0.2955(3) 0.0288(9) Uani 1 1 d . . . . .
H10 H 0.891043 0.872998 0.318950 0.035 Uiso 1 1 calc R U . . .
C9 C 0.7035(5) 0.8618(5) 0.2314(3) 0.0240(9) Uani 1 1 d . . . . .
C1 C 0.3128(5) 0.2918(5) 0.0299(3) 0.0265(9) Uani 1 1 d . . . . .
C7 C 0.3638(5) 0.4376(5) 0.0606(3) 0.0258(9) Uani 1 1 d . . . . .
H7 H 0.301798 0.484828 0.039331 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8920(5) 1.0670(5) 0.3245(3) 0.0329(10) Uani 1 1 d . . . . .
H11 H 0.983944 1.111766 0.367506 0.040 Uiso 1 1 calc R U . . .
C6 C 0.1764(5) 0.2253(6) -0.0340(3) 0.0339(11) Uani 1 1 d . . . . .
H6 H 0.121589 0.279305 -0.054099 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6855(5) 1.0831(5) 0.2314(3) 0.0309(10) Uani 1 1 d . . . . .
H12 H 0.633771 1.139077 0.210454 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3915(5) 0.2093(5) 0.0591(3) 0.0293(10) Uani 1 1 d . . . . .
C3 C 0.3365(6) 0.0672(5) 0.0237(4) 0.0383(12) Uani 1 1 d . . . . .
H3A H 0.391498 0.012459 0.042268 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1199(6) 0.0841(6) -0.0682(4) 0.0394(12) Uani 1 1 d . . . . .
H5 H 0.027401 0.041760 -0.110913 0.047 Uiso 1 1 calc R U . . .
C4 C 0.2006(6) 0.0050(5) -0.0392(4) 0.0370(11) Uani 1 1 d . . . . .
C14 C 0.0185(9) -0.2131(8) -0.1310(6) 0.070(2) Uani 1 1 d . . . . .
H14A H 0.002598 -0.178230 -0.184042 0.106 Uiso 1 1 calc R U . . .
H14B H -0.053928 -0.206151 -0.101917 0.106 Uiso 1 1 calc R U . . .
H14C H 0.011693 -0.309406 -0.148765 0.106 Uiso 1 1 calc R U . . .
H3 H 0.846(5) 1.229(2) 0.306(3) 0.022(13) Uiso 1 1 d D . . . .
N4 N 0.000000 0.500000 0.000000 0.074(3) Uani 1 2 d DS U P A 1
C15 C 0.0877(11) 0.6020(9) 0.0470(9) 0.056(2) Uani 0.5 1 d D U P A 1
C16 C 0.2079(12) 0.7305(10) 0.0930(10) 0.056(2) Uani 0.5 1 d D U P A 1
H16A H 0.220230 0.787492 0.051379 0.083 Uiso 0.5 1 calc R U P A 1
H16B H 0.295407 0.709609 0.114408 0.083 Uiso 0.5 1 calc R U P A 1
H16C H 0.188537 0.780170 0.143869 0.083 Uiso 0.5 1 calc R U P A 1
N5 N 0.2844(7) 0.5030(8) 0.2497(5) 0.0748(15) Uani 1 1 d . . . . .
C17 C 0.1985(9) 0.5517(10) 0.2423(6) 0.0748(15) Uani 1 1 d . . . . .
C18A C 0.0977(17) 0.6437(19) 0.2110(12) 0.0748(15) Uani 0.5 1 d . . P B 2
H18A H 0.136875 0.697196 0.173036 0.112 Uiso 0.5 1 calc R U P B 2
H18B H 0.096689 0.706260 0.264023 0.112 Uiso 0.5 1 calc R U P B 2
H18C H 0.000014 0.582090 0.177379 0.112 Uiso 0.5 1 calc R U P B 2
C18 C 0.0819(17) 0.5742(19) 0.2633(12) 0.0748(15) Uani 0.5 1 d . . P B 1
H18D H -0.005345 0.497150 0.227635 0.112 Uiso 0.5 1 calc R U P B 1
H18E H 0.073590 0.659524 0.250144 0.112 Uiso 0.5 1 calc R U P B 1
H18F H 0.095147 0.581901 0.327031 0.112 Uiso 0.5 1 calc R U P B 1
O21 O 1.0159(8) 1.3955(10) 0.4240(7) 0.0320(18) Uani 0.5 1 d G . P C 1
H21A H 0.948594 1.408334 0.444973 0.048 Uiso 0.5 1 d G U P C 1
H21B H 1.031646 1.456143 0.393834 0.048 Uiso 0.5 1 d G U P C 1
O21A O 1.0502(12) 1.3807(9) 0.3840(8) 0.048(2) Uani 0.5 1 d G . P D 2
H21C H 1.132955 1.387163 0.376810 0.072 Uiso 0.5 1 d G U P D 2
H21D H 1.068077 1.405244 0.441717 0.072 Uiso 0.5 1 d G U P D 2
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_
_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
O12 Mo3 Mo4 124.55(8) . . ?
O12 Mo3 O11 79.33(11) . . ?
O12 Mo3 O11 77.26(10) . 2_676 ?
O12 Mo3 O13 149.93(12) . . ?
O11 Mo3 Mo4 45.23(7) . . ?
O11 Mo3 Mo4 86.36(6) 2_676 . ?
O11 Mo3 O11 75.63(11) . 2_676 ?
O13 Mo3 Mo4 36.61(8) . . ?
O13 Mo3 O11 78.12(11) . . ?
O13 Mo3 O11 78.06(10) . 2_676 ?
O17 Mo3 Mo4 132.89(10) . . ?
O17 Mo3 O12 96.63(13) . . ?
O17 Mo3 O11 156.77(12) . . ?
O17 Mo3 O11 81.16(11) . 2_676 ?
O17 Mo3 O13 96.28(13) . . ?
O8 Mo3 Mo4 89.39(11) . . ?
O8 Mo3 O12 101.02(13) . . ?
O8 Mo3 O11 97.70(13) . . ?
O8 Mo3 O11 173.29(12) . 2_676 ?
O8 Mo3 O13 101.49(13) . . ?
O8 Mo3 O17 105.52(14) . . ?
O12 Mo2 O11 73.32(10) . . ?
O12 Mo2 O13 72.17(10) . 2_676 ?
O15 Mo2 O12 146.74(12) . . ?
O15 Mo2 O11 77.66(11) . . ?
O15 Mo2 O13 83.63(11) . 2_676 ?
O13 Mo2 O11 71.66(10) 2_676 . ?
O7 Mo2 O12 96.44(13) . . ?
O7 Mo2 O11 92.22(12) . . ?
O7 Mo2 O15 100.61(14) . . ?
O7 Mo2 O13 162.21(12) . 2_676 ?
O16 Mo2 O12 101.42(13) . . ?
O16 Mo2 O11 162.43(13) . . ?
O16 Mo2 O15 101.37(14) . . ?
O16 Mo2 O13 90.78(13) . 2_676 ?
O16 Mo2 O7 105.12(15) . . ?
O12 Mo4 Mo3 79.45(7) 2_676 . ?
O14 Mo4 Mo3 121.30(9) . . ?
O14 Mo4 O12 84.54(11) . 2_676 ?
O14 Mo4 O11 79.10(11) . . ?
O14 Mo4 O13 148.67(12) . . ?
O11 Mo4 Mo3 42.22(7) . . ?
O11 Mo4 O12 72.16(10) . 2_676 ?
O13 Mo4 Mo3 35.76(8) . . ?
O13 Mo4 O12 71.61(10) . 2_676 ?
O13 Mo4 O11 74.49(10) . . ?
O9 Mo4 Mo3 85.20(11) . . ?
O9 Mo4 O12 164.36(13) . 2_676 ?
O9 Mo4 O14 101.06(15) . . ?
O9 Mo4 O11 94.40(13) . . ?
O9 Mo4 O13 97.51(14) . . ?
O9 Mo4 O18 104.85(17) . . ?
O18 Mo4 Mo3 135.44(11) . . ?
O18 Mo4 O12 88.38(13) . 2_676 ?
O18 Mo4 O14 99.61(15) . . ?
O18 Mo4 O11 160.54(14) . . ?
O18 Mo4 O13 99.73(14) . . ?
O14 Mo5 O11 73.35(11) . . ?
O14 Mo5 O17 77.90(12) . 2_676 ?
O15 Mo5 O14 144.89(12) . . ?
O15 Mo5 O11 74.50(10) . . ?
O15 Mo5 O17 77.93(12) . 2_676 ?
O17 Mo5 O11 69.39(10) 2_676 . ?
O10 Mo5 O14 97.37(15) . . ?
O10 Mo5 O11 93.33(13) . . ?
O10 Mo5 O15 98.19(15) . . ?
O10 Mo5 O17 162.71(13) . 2_676 ?
O19 Mo5 O14 103.01(15) . . ?
O19 Mo5 O11 161.36(14) . . ?
O19 Mo5 O15 102.90(15) . . ?
O19 Mo5 O17 91.98(14) . 2_676 ?
O19 Mo5 O10 105.30(17) . . ?
O2 Mo1 O5 79.31(13) . . ?
O2 Mo1 N1 72.18(13) . . ?
O1 Mo1 O5 81.86(15) . . ?
O1 Mo1 O2 150.84(15) . . ?
O1 Mo1 N1 82.01(14) . . ?
O4 Mo1 O5 81.17(18) . . ?
O4 Mo1 O2 98.01(16) . . ?
O4 Mo1 O1 100.88(16) . . ?
O4 Mo1 N1 157.24(19) . . ?
O3 Mo1 O5 172.51(15) . . ?
O3 Mo1 O2 96.42(18) . . ?
O3 Mo1 O1 99.6(2) . . ?
O3 Mo1 O4 105.6(2) . . ?
O3 Mo1 N1 95.99(16) . . ?
N1 Mo1 O5 76.89(13) . . ?
Mo3 O12 Mo2 109.61(12) . . ?
Mo3 O12 Mo4 109.49(12) . 2_676 ?
Mo2 O12 Mo4 103.44(12) . 2_676 ?
Mo4 O14 Mo5 115.64(15) . . ?
Mo3 O11 Mo3 104.38(11) . 2_676 ?
Mo3 O11 Mo2 91.22(10) . . ?
Mo3 O11 Mo2 96.40(9) 2_676 . ?
Mo3 O11 Mo4 92.56(10) . . ?
Mo3 O11 Mo5 164.00(13) . . ?
Mo3 O11 Mo5 91.50(9) 2_676 . ?
Mo2 O11 Mo5 84.94(9) . . ?
Mo4 O11 Mo3 98.37(10) . 2_676 ?
Mo4 O11 Mo2 163.33(13) . . ?
Mo4 O11 Mo5 86.99(9) . . ?
Mo2 O15 Mo5 117.69(14) . . ?
Mo3 O13 Mo2 111.19(12) . 2_676 ?
Mo3 O13 Mo4 107.62(12) . . ?
Mo4 O13 Mo2 104.31(12) . 2_676 ?
Mo3 O17 Mo5 117.93(14) . 2_676 ?
Mo1 O5 H5A 111.4 . . ?
Mo1 O5 H5B 111.4 . . ?
H5A O5 H5B 102.5 . . ?
C8 O2 Mo1 118.4(3) . . ?
C2 O1 Mo1 137.1(3) . . ?
H20A O20 H20B 104.5 . . ?
N2 N1 Mo1 115.0(3) . . ?
C7 N1 Mo1 129.2(3) . . ?
C7 N1 N2 115.8(4) . . ?
C11 N3 C12 122.5(4) . . ?
C11 N3 H3 124(4) . . ?
C12 N3 H3 113(4) . . ?
N1 N2 H2 125.3 . . ?
C8 N2 N1 109.4(4) . . ?
C8 N2 H2 125.3 . . ?
C9 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C9 119.4(4) . . ?
C4 O6 C14 123.1(6) . . ?
O2 C8 C9 116.4(4) . . ?
N2 C8 O2 123.9(4) . . ?
N2 C8 C9 119.6(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C11 C10 C9 119.4(4) . . ?
C13 C9 C8 120.9(4) . . ?
C13 C9 C10 119.0(4) . . ?
C10 C9 C8 120.1(4) . . ?
C6 C1 C7 118.5(4) . . ?
C2 C1 C7 123.7(4) . . ?
C2 C1 C6 117.8(5) . . ?
N1 C7 C1 123.9(4) . . ?
N1 C7 H7 118.0 . . ?
C1 C7 H7 118.0 . . ?
N3 C11 C10 120.0(4) . . ?
N3 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C1 C6 H6 118.9 . . ?
C5 C6 C1 122.2(5) . . ?
C5 C6 H6 118.9 . . ?
N3 C12 C13 119.7(4) . . ?
N3 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
O1 C2 C1 122.7(4) . . ?
O1 C2 C3 116.8(5) . . ?
C3 C2 C1 120.4(5) . . ?
C2 C3 H3A 119.9 . . ?
C2 C3 C4 120.1(5) . . ?
C4 C3 H3A 119.9 . . ?
C6 C5 H5 120.5 . . ?
C6 C5 C4 118.9(5) . . ?
C4 C5 H5 120.5 . . ?
O6 C4 C3 116.2(5) . . ?
O6 C4 C5 123.3(5) . . ?
C5 C4 C3 120.6(5) . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 N4 C15 180.0 . 2_565 ?
N4 C15 C16 170.1(16) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 C18A 162.5(12) . . ?
N5 C17 C18 151.5(15) . . ?
C17 C18A H18A 109.5 . . ?
C17 C18A H18B 109.5 . . ?
C17 C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C17 C18 H18D 109.5 . . ?
C17 C18 H18E 109.5 . . ?
C17 C18 H18F 109.5 . . ?
H18D C18 H18E 109.5 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
H21A O21 H21B 104.5 . . ?
H21C O21A H21D 104.5 . . ?
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
Mo3 Mo4 3.1933(4) . ?
Mo3 O12 1.953(3) . ?
Mo3 O11 2.346(3) 2_676 ?
Mo3 O11 2.148(3) . ?
Mo3 O13 1.958(3) . ?
Mo3 O17 1.753(3) . ?
Mo3 O8 1.689(3) . ?
Mo2 O12 1.998(3) . ?
Mo2 O11 2.365(3) . ?
Mo2 O15 1.898(3) . ?
Mo2 O13 2.293(3) 2_676 ?
Mo2 O7 1.710(3) . ?
Mo2 O16 1.705(3) . ?
Mo4 O12 2.317(3) 2_676 ?
Mo4 O14 1.911(3) . ?
Mo4 O11 2.269(3) . ?
Mo4 O13 1.998(3) . ?
Mo4 O9 1.695(3) . ?
Mo4 O18 1.713(3) . ?
Mo5 O14 1.951(3) . ?
Mo5 O11 2.475(3) . ?
Mo5 O15 1.922(3) . ?
Mo5 O17 2.267(3) 2_676 ?
Mo5 O10 1.710(3) . ?
Mo5 O19 1.690(3) . ?
Mo1 O5 2.371(4) . ?
Mo1 O2 2.011(3) . ?
Mo1 O1 1.932(3) . ?
Mo1 O4 1.710(3) . ?
Mo1 O3 1.688(4) . ?
Mo1 N1 2.225(4) . ?
O5 H5A 0.9107 . ?
O5 H5B 0.9108 . ?
O2 C8 1.323(5) . ?
O1 C2 1.344(6) . ?
O20 H20A 0.8700 . ?
O20 H20B 0.8699 . ?
N1 N2 1.400(5) . ?
N1 C7 1.296(6) . ?
N3 C11 1.335(7) . ?
N3 C12 1.341(6) . ?
N3 H3 0.861(19) . ?
N2 H2 0.8800 . ?
N2 C8 1.287(6) . ?
C13 H13 0.9500 . ?
C13 C9 1.389(6) . ?
C13 C12 1.376(7) . ?
O6 C4 1.364(7) . ?
O6 C14 1.410(9) . ?
C8 C9 1.474(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.395(6) . ?
C10 C11 1.372(7) . ?
C1 C7 1.421(7) . ?
C1 C6 1.410(7) . ?
C1 C2 1.409(7) . ?
C7 H7 0.9500 . ?
C11 H11 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.382(8) . ?
C12 H12 0.9500 . ?
C2 C3 1.392(7) . ?
C3 H3A 0.9500 . ?
C3 C4 1.397(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.392(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N4 C15 1.167(7) 2_565 ?
N4 C15 1.167(7) . ?
C15 C16 1.466(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N5 C17 1.131(11) . ?
C17 C18A 1.66(2) . ?
C17 C18 1.388(18) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C18 H18D 0.9800 . ?
C18 H18E 0.9800 . ?
C18 H18F 0.9800 . ?
O21 H21A 0.8698 . ?
O21 H21B 0.8701 . ?
O21A H21C 0.8701 . ?
O21A H21D 0.8700 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo4 Mo3 O17 Mo5 75.30(18) . . . 2_676 ?
Mo1 O2 C8 N2 9.8(6) . . . . ?
Mo1 O2 C8 C9 -169.5(3) . . . . ?
Mo1 O1 C2 C1 -15.2(8) . . . . ?
Mo1 O1 C2 C3 165.8(4) . . . . ?
Mo1 N1 N2 C8 -6.2(4) . . . . ?
Mo1 N1 C7 C1 0.4(7) . . . . ?
O12 Mo3 O17 Mo5 -77.23(16) . . . 2_676 ?
O12 Mo2 O15 Mo5 50.8(3) . . . . ?
O11 Mo3 O17 Mo5 1.1(4) . . . 2_676 ?
O11 Mo3 O17 Mo5 -1.27(13) 2_676 . . 2_676 ?
O11 Mo2 O15 Mo5 21.19(15) . . . . ?
O13 Mo3 O17 Mo5 75.56(16) . . . 2_676 ?
O13 Mo2 O15 Mo5 93.75(16) 2_676 . . . ?
O7 Mo2 O15 Mo5 -68.77(19) . . . . ?
O8 Mo3 O17 Mo5 179.36(15) . . . 2_676 ?
O16 Mo2 O15 Mo5 -176.74(17) . . . . ?
O2 C8 C9 C13 -178.5(4) . . . . ?
O2 C8 C9 C10 1.0(6) . . . . ?
O1 C2 C3 C4 176.9(5) . . . . ?
N1 N2 C8 O2 -1.7(6) . . . . ?
N1 N2 C8 C9 177.6(4) . . . . ?
N2 N1 C7 C1 179.7(4) . . . . ?
N2 C8 C9 C13 2.2(7) . . . . ?
N2 C8 C9 C10 -178.3(4) . . . . ?
C9 C13 C12 N3 0.9(7) . . . . ?
C9 C10 C11 N3 1.0(7) . . . . ?
C1 C6 C5 C4 -0.5(8) . . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C7 N1 N2 C8 174.4(4) . . . . ?
C7 C1 C6 C5 179.0(5) . . . . ?
C7 C1 C2 O1 3.3(7) . . . . ?
C7 C1 C2 C3 -177.8(5) . . . . ?
C11 N3 C12 C13 -0.7(7) . . . . ?
C11 C10 C9 C13 -0.8(7) . . . . ?
C11 C10 C9 C8 179.7(4) . . . . ?
C6 C1 C7 N1 -176.7(5) . . . . ?
C6 C1 C2 O1 -177.2(5) . . . . ?
C6 C1 C2 C3 1.7(7) . . . . ?
C6 C5 C4 O6 -178.3(5) . . . . ?
C6 C5 C4 C3 0.2(8) . . . . ?
C12 N3 C11 C10 -0.2(8) . . . . ?
C12 C13 C9 C8 179.4(4) . . . . ?
C12 C13 C9 C10 -0.2(7) . . . . ?
C2 C1 C7 N1 2.8(7) . . . . ?
C2 C1 C6 C5 -0.5(8) . . . . ?
C2 C3 C4 O6 179.6(5) . . . . ?
C2 C3 C4 C5 1.1(8) . . . . ?
C14 O6 C4 C3 176.6(6) . . . . ?
C14 O6 C4 C5 -4.9(10) . . . . ?
