#------------------------------------------------------------------------------
#$Date: 2021-10-06 17:51:35 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269676 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/32/7243287.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_7243287
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, 4(C13 H12 Mo N3 O6), 10(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H74 Mo12 N14 O60'
_chemical_formula_weight         3054.57
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-4-hydroxybenzylidene)isonicotinylhydrazonium)-molybdenum(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             2021-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                116.276(3)
_cell_angle_beta                 95.232(3)
_cell_angle_gamma                93.035(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4085(4)
_cell_length_b                   16.2433(5)
_cell_length_c                   17.3878(4)
_cell_measurement_reflns_used    23681
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.7510
_cell_measurement_theta_min      3.0260
_cell_volume                     2359.80(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     28.00 121.00   0.50    0.10    --   47.77  72.00-138.00  186
  2  ω    116.00 178.00   0.50    0.15    --  113.25  72.00-138.00  124
  3  ω    101.00 178.00   0.50    0.15    --  113.25  45.00-150.00  154
  4  ω    101.00 173.00   0.50    0.15    --  113.25  45.00 -90.00  144
  5  ω    143.00 178.00   0.50    0.15    --  113.25  30.00-180.00   70
  6  ω    104.00 174.00   0.50    0.15    --  113.25  45.00 -60.00  140
  7  ω    101.00 135.00   0.50    0.15    --  113.25  30.00   0.00   68
  8  ω    139.00 178.00   0.50    0.15    --  113.25  30.00  60.00   78
  9  ω    130.00 165.00   0.50    0.15    --  113.25  45.00  90.00   70
 10  ω    103.00 128.00   0.50    0.15    --  113.25  30.00  60.00   50
 11  ω    100.00 175.00   0.50    0.15    --  113.25  15.00 150.00  150
 12  ω    118.00 172.00   0.50    0.15    --  113.25  15.00  30.00  108
 13  ω    142.00 168.00   0.50    0.15    --  113.25  30.00   0.00   52
 14  ω    101.00 126.00   0.50    0.15    --  113.25  30.00-180.00   50
 15  ω    -68.00 -25.00   0.50    0.10    --  -47.77  72.00-138.00   86
 16  ω    -79.00 -54.00   0.50    0.15    --  -91.75  72.00-138.00   50
 17  ω    -16.00  11.00   0.50    0.10    --  -47.77  72.00-138.00   54
 18  ω    -50.00 -20.00   0.50    0.15    --  -91.75  45.00   0.00   60
 19  ω    -51.00 -20.00   0.50    0.15    --  -91.75  45.00  30.00   62
 20  ω     88.00 130.00   0.50    0.15    --  113.25-151.00-132.23   84
 21  ω     36.00  81.00   0.50    0.10    --   47.77-125.00 -60.00   90
 22  ω     76.00 101.00   0.50    0.15    --  113.25-125.00  30.00   50
 23  ω     42.00  68.00   0.50    0.15    --  113.25-125.00  30.00   52
 24  ω     72.00  98.00   0.50    0.15    --  113.25-125.00 -30.00   52
 25  ω     43.00  81.00   0.50    0.15    --  113.25-125.00 -60.00   76
 26  ω     52.00 110.00   0.50    0.15    --  113.25-125.00-120.00  116
 27  ω     51.00 106.00   0.50    0.15    --  113.25-108.00 -64.43  110
 28  ω     55.00 122.00   0.50    0.15    --  113.25-139.00   9.82  134
 29  ω     85.00 111.00   0.50    0.15    --  113.25-125.00  60.00   52
 30  ω     86.00 111.00   0.50    0.15    --  113.25-125.00 150.00   50
 31  ω     48.00 111.00   0.50    0.15    --  113.25-125.00 120.00  126
 32  ω     46.00  72.00   0.50    0.15    --  113.25 -95.00  60.00   52
 33  ω     76.00 102.00   0.50    0.15    --  113.25 -95.00  90.00   52
 34  ω     47.00  85.00   0.50    0.15    --  113.25 -95.00   0.00   76
 35  ω     78.00 106.00   0.50    0.15    --  113.25 -95.00  30.00   56
 36  ω     43.00 106.00   0.50    0.15    --  113.25 -95.00 150.00  126
 37  ω     43.00  75.00   0.50    0.15    --  113.25 -95.00  30.00   64
 38  ω     47.00 108.00   0.50    0.15    --  113.25-108.00-115.90  122
 39  ω     64.00 103.00   0.50    0.15    --  113.25 -95.00 -30.00   78
 40  ω     69.00 106.00   0.50    0.15    --  113.25 -95.00-150.00   74
 41  ω     81.00 106.00   0.50    0.15    --  113.25 -95.00-180.00   50
 42  ω     46.00  76.00   0.50    0.15    --  113.25 -95.00-180.00   60
 43  ω     68.00  94.00   0.50    0.15    --  113.25 -77.00-150.00   52
 44  ω     42.00  67.00   0.50    0.15    --  113.25 -61.00-150.00   50
 45  ω     45.00  71.00   0.50    0.15    --  113.25 -61.00  30.00   52
 46  ω     42.00  93.00   0.50    0.15    --  113.25 -77.00  90.00  102
 47  ω     42.00  67.00   0.50    0.15    --  113.25 -72.00  91.00   50
 48  ω     44.00  70.00   0.50    0.15    --  113.25 -61.00  90.00   52
 49  ω     11.00  65.00   0.50    0.10    --   47.77 -72.00  91.00  108
 50  ω     44.00  70.00   0.50    0.15    --  113.25 -61.00 -30.00   52
 51  ω     46.00  71.00   0.50    0.15    --  113.25 -61.00 -90.00   50
 52  ω     96.00 128.00   0.50    0.15    --  113.25 125.00-180.00   64
 53  ω    140.00 165.00   0.50    0.15    --  113.25 125.00-180.00   50
 54  ω     97.00 168.00   0.50    0.15    --  113.25 125.00 -60.00  142
 55  ω    -68.00 -14.00   0.50    0.10    --  -47.77 125.00 120.00  108
 56  ω    -77.00 -18.00   0.50    0.10    --  -47.77 125.00   0.00  118
 57  ω   -118.00 -28.00   0.50    0.10    --  -47.77 -72.00  91.00  180
 58  ω   -141.00-115.00   0.50    0.15    --  -91.75 -72.00  91.00   52
 59  ω   -102.00 -73.00   0.50    0.10    --  -47.77-125.00-120.00   58
 60  ω   -115.00 -89.00   0.50    0.10    --  -47.77-125.00-150.00   52
;
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.466
_diffrn_reflns_theta_min         2.858
_exptl_absorpt_coefficient_mu    13.601
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.114
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.719
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.00031(4)
_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   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0764P)²+17.1814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9372
_reflns_number_total             10049
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_947_auto
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_database_code               7243287
_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   0.612
_shelx_estimated_absorpt_t_min   0.091
_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) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(Mo3)
3.a Free rotating group:
 O24(H24A,H24B), O20(H20A,H20B), O23(H23A,H23B), O22(H22A,H22B), O21(H21A,H21B)
3.b Rotating group:
 O5A(H5AA,H5AB), O5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N3A(H3AA), C6(H6A), C3A(H3AB), C10(H10), C13(H13), C5(H5), C12(H12),
 C11(H11), C6A(H6AB), C7(H7), C7A(H7A), C5A(H5AC), C10A(H10A), C3(H3A),
 C11A(H11A), C13A(H13A), C12A(H12A)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
3.e Idealised tetrahedral OH refined as rotating group:
 O6A(H6AA), O6(H6)
;
_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 1.14747(4) 0.98836(3) 0.93898(3) 0.01658(12) Uani 1 1 d . . . . .
Mo4 Mo 0.85594(5) 0.86112(3) 0.84244(3) 0.02019(13) Uani 1 1 d . . . . .
Mo5 Mo 0.68576(5) 1.04356(3) 0.89228(3) 0.02165(13) Uani 1 1 d . . . . .
Mo1 Mo 0.59996(5) 0.22450(3) 0.55070(3) 0.02229(13) Uani 1 1 d . . . . .
Mo1A Mo 0.09780(5) 0.32057(3) 0.51704(3) 0.02174(13) Uani 1 1 d . . . . .
Mo2 Mo 0.98371(5) 1.17462(3) 0.99351(3) 0.01915(12) Uani 1 1 d . . . . .
O13 O 1.0523(4) 0.8630(3) 0.8965(2) 0.0185(8) Uani 1 1 d . . . . .
O2 O 0.7492(5) 0.1517(3) 0.4802(3) 0.0250(9) Uani 1 1 d . . . . .
O15 O 0.7804(4) 1.1622(3) 0.9745(3) 0.0217(8) Uani 1 1 d . . . . .
O2A O -0.0408(4) 0.2792(3) 0.4091(3) 0.0243(8) Uani 1 1 d . . . . .
O17 O 1.3089(4) 0.9664(3) 0.9813(3) 0.0218(8) Uani 1 1 d . . . . .
O1 O 0.4975(5) 0.2624(3) 0.6494(3) 0.0269(9) Uani 1 1 d . . . . .
O7 O 1.0301(5) 1.1699(3) 0.8980(3) 0.0256(9) Uani 1 1 d . . . . .
O14 O 0.6771(5) 0.9115(3) 0.8534(3) 0.0262(9) Uani 1 1 d . . . . .
O12 O 1.1602(4) 1.1204(3) 1.0187(3) 0.0206(8) Uani 1 1 d . . . . .
O11 O 0.9246(4) 1.0114(3) 0.9330(2) 0.01658(12) Uani 1 1 d . . . . .
O5A O 0.2404(5) 0.2413(3) 0.4087(3) 0.0267(9) Uani 1 1 d . . . . .
H5AA H 0.186411 0.198085 0.363636 0.040 Uiso 1 1 d GR . . . .
H5AB H 0.299091 0.211063 0.426136 0.040 Uiso 1 1 d GR . . . .
O1A O 0.2871(5) 0.3724(3) 0.5766(3) 0.0268(9) Uani 1 1 d . . . . .
O8 O 1.1825(5) 0.9891(3) 0.8458(3) 0.0235(8) Uani 1 1 d . . . . .
O6A O 0.6654(5) 0.5824(3) 0.7643(3) 0.0304(10) Uani 1 1 d . . . . .
H6AA H 0.709142 0.634346 0.777916 0.046 Uiso 1 1 calc GR . . . .
O16 O 1.0244(5) 1.2863(3) 1.0668(3) 0.0304(10) Uani 1 1 d . . . . .
O5 O 0.7928(5) 0.2753(3) 0.6623(3) 0.0320(10) Uani 1 1 d . . . . .
H5A H 0.772029 0.258207 0.701264 0.048 Uiso 1 1 d GR . . . .
H5B H 0.802390 0.335441 0.689496 0.048 Uiso 1 1 d GR . . . .
O10 O 0.7286(5) 1.0469(3) 0.8000(3) 0.0290(9) Uani 1 1 d . . . . .
O19 O 0.5097(5) 1.0619(4) 0.8942(3) 0.0311(10) Uani 1 1 d . . . . .
O9 O 0.9025(5) 0.8669(3) 0.7524(3) 0.0287(9) Uani 1 1 d . . . . .
O6 O 0.1797(5) 0.2859(3) 0.8475(3) 0.0335(10) Uani 1 1 d . . . . .
H6 H 0.129732 0.251425 0.861352 0.050 Uiso 1 1 calc GR . . . .
O4A O 0.0795(5) 0.2209(3) 0.5266(3) 0.0333(10) Uani 1 1 d . . . . .
O24 O -0.5769(5) 0.2177(4) 0.0293(3) 0.0351(11) Uani 1 1 d . . . . .
H24A H -0.653254 0.196147 0.041875 0.053 Uiso 1 1 d G . . . .
H24B H -0.555827 0.171577 -0.016905 0.053 Uiso 1 1 d G . . . .
O4 O 0.6527(6) 0.3267(3) 0.5505(3) 0.0342(11) Uani 1 1 d . . . . .
O18 O 0.7966(5) 0.7468(3) 0.8084(3) 0.0319(10) Uani 1 1 d . . . . .
N1A N 0.1407(5) 0.4156(3) 0.4578(3) 0.0219(10) Uani 1 1 d . . . . .
O20 O 0.7971(5) 0.2299(4) 0.7991(3) 0.0319(10) Uani 1 1 d . . . . .
H20A H 0.728289 0.202492 0.812344 0.048 Uiso 1 1 d G . . . .
H20B H 0.830956 0.277314 0.847684 0.048 Uiso 1 1 d G . . . .
O3A O -0.0013(6) 0.3954(4) 0.5890(3) 0.0386(11) Uani 1 1 d . . . . .
O23 O -0.1119(6) 0.4640(4) 0.7407(3) 0.0414(12) Uani 1 1 d . . . . .
H23A H -0.084562 0.460959 0.693203 0.062 Uiso 1 1 d G . . . .
H23B H -0.192288 0.488833 0.744811 0.062 Uiso 1 1 d G . . . .
N3 N 1.0292(5) -0.0973(4) 0.3010(3) 0.0236(10) Uani 1 1 d . . . . .
H3 H 1.082483 -0.133328 0.263290 0.028 Uiso 1 1 calc R . . . .
N1 N 0.6269(5) 0.1039(3) 0.5784(3) 0.0217(10) Uani 1 1 d . . . . .
N2 N 0.7164(5) 0.0412(3) 0.5275(3) 0.0204(9) Uani 1 1 d . . . . .
O3 O 0.4604(6) 0.1725(4) 0.4707(3) 0.0396(12) Uani 1 1 d . . . . .
N2A N 0.0503(5) 0.3978(3) 0.3826(3) 0.0226(10) Uani 1 1 d . . . . .
O22 O 0.9163(7) 0.4988(5) 1.1097(4) 0.0470(13) Uani 1 1 d . . . . .
H22A H 0.972071 0.507772 1.156051 0.071 Uiso 1 1 d G . . . .
H22B H 0.829855 0.494583 1.122480 0.071 Uiso 1 1 d G . . . .
N3A N -0.3660(6) 0.2464(4) 0.1558(4) 0.0338(13) Uani 1 1 d . . . . .
H3AA H -0.435819 0.229957 0.112943 0.041 Uiso 1 1 calc R . . . .
C9 C 0.8642(6) 0.0140(4) 0.4171(4) 0.0218(11) Uani 1 1 d . . . . .
C1 C 0.4706(6) 0.1373(4) 0.6879(4) 0.0217(11) Uani 1 1 d . . . . .
O21 O 0.9292(9) 0.3759(4) 0.9338(4) 0.0581(17) Uani 1 1 d . . . . .
H21A H 0.969532 0.413604 0.917054 0.087 Uiso 1 1 d G . . . .
H21B H 0.931556 0.408391 0.989421 0.087 Uiso 1 1 d G . . . .
C4A C 0.5592(6) 0.5621(4) 0.6982(4) 0.0230(11) Uani 1 1 d . . . . .
C9A C -0.1522(6) 0.2980(4) 0.2901(4) 0.0220(11) Uani 1 1 d . . . . .
C2 C 0.4359(6) 0.2239(4) 0.6944(4) 0.0231(11) Uani 1 1 d . . . . .
C8 C 0.7715(6) 0.0722(4) 0.4788(4) 0.0196(11) Uani 1 1 d . . . . .
C6 C 0.4084(7) 0.1055(4) 0.7414(4) 0.0228(11) Uani 1 1 d . . . . .
H6A H 0.432971 0.048867 0.739842 0.027 Uiso 1 1 calc R . . . .
C3A C 0.4714(6) 0.4795(4) 0.6701(4) 0.0235(12) Uani 1 1 d . . . . .
H3AB H 0.486357 0.440715 0.697262 0.028 Uiso 1 1 calc R . . . .
C10 C 0.9268(6) 0.0424(4) 0.3629(4) 0.0224(11) Uani 1 1 d . . . . .
H10 H 0.913420 0.101497 0.366414 0.027 Uiso 1 1 calc R . . . .
C13 C 0.8870(6) -0.0727(4) 0.4121(4) 0.0215(11) Uani 1 1 d . . . . .
H13 H 0.844298 -0.093254 0.448859 0.026 Uiso 1 1 calc R . . . .
C8A C -0.0409(7) 0.3280(4) 0.3653(4) 0.0228(11) Uani 1 1 d . . . . .
C5 C 0.3127(6) 0.1539(4) 0.7963(4) 0.0237(12) Uani 1 1 d . . . . .
H5 H 0.271841 0.131192 0.832100 0.028 Uiso 1 1 calc R . . . .
C4 C 0.2773(7) 0.2374(4) 0.7978(4) 0.0254(12) Uani 1 1 d . . . . .
C12 C 0.9719(7) -0.1277(4) 0.3534(4) 0.0249(12) Uani 1 1 d . . . . .
H12 H 0.989949 -0.186190 0.349781 0.030 Uiso 1 1 calc R . . . .
C11 C 1.0094(7) -0.0157(4) 0.3032(4) 0.0261(12) Uani 1 1 d . . . . .
H11 H 1.051160 0.002408 0.264615 0.031 Uiso 1 1 calc R . . . .
C1A C 0.3417(6) 0.5111(4) 0.5603(4) 0.0219(11) Uani 1 1 d . . . . .
C6A C 0.4345(7) 0.5931(4) 0.5899(4) 0.0248(12) Uani 1 1 d . . . . .
H6AB H 0.423068 0.631267 0.561761 0.030 Uiso 1 1 calc R . . . .
C7 C 0.5657(6) 0.0815(4) 0.6307(4) 0.0211(11) Uani 1 1 d . . . . .
H7 H 0.584519 0.024950 0.631540 0.025 Uiso 1 1 calc R . . . .
C7A C 0.2356(6) 0.4867(4) 0.4864(4) 0.0213(11) Uani 1 1 d . . . . .
H7A H 0.235330 0.524367 0.457361 0.026 Uiso 1 1 calc R . . . .
C5A C 0.5401(7) 0.6191(4) 0.6578(4) 0.0252(12) Uani 1 1 d . . . . .
H5AC H 0.600099 0.675294 0.677327 0.030 Uiso 1 1 calc R . . . .
C10A C -0.2551(7) 0.2238(5) 0.2704(4) 0.0306(14) Uani 1 1 d . . . . .
H10A H -0.252235 0.190690 0.303872 0.037 Uiso 1 1 calc R . . . .
C3 C 0.3402(7) 0.2730(4) 0.7483(4) 0.0257(12) Uani 1 1 d . . . . .
H3A H 0.317390 0.330676 0.751489 0.031 Uiso 1 1 calc R . . . .
C11A C -0.3598(7) 0.1997(5) 0.2023(5) 0.0333(14) Uani 1 1 d . . . . .
H11A H -0.429243 0.148854 0.187778 0.040 Uiso 1 1 calc R . . . .
C2A C 0.3629(6) 0.4546(4) 0.6026(4) 0.0220(11) Uani 1 1 d . . . . .
C13A C -0.1619(7) 0.3452(5) 0.2401(5) 0.0327(14) Uani 1 1 d . . . . .
H13A H -0.094456 0.396550 0.252607 0.039 Uiso 1 1 calc R . . . .
C12A C -0.2705(8) 0.3167(5) 0.1721(5) 0.0363(15) Uani 1 1 d . . . . .
H12A H -0.276860 0.347603 0.136835 0.044 Uiso 1 1 calc R . . . .
N4 N 0.5970(10) 0.4806(7) 1.1072(6) 0.065(2) Uani 1 1 d . . . . .
C14 C 0.4773(11) 0.4619(7) 1.0828(6) 0.055(2) Uani 1 1 d . . . . .
C15 C 0.3231(14) 0.4428(10) 1.0551(8) 0.078(3) Uani 1 1 d . . . . .
H15A H 0.304996 0.421160 0.992446 0.117 Uiso 1 1 calc GR . . . .
H15B H 0.277032 0.499348 1.084623 0.117 Uiso 1 1 calc GR . . . .
H15C H 0.283760 0.395128 1.069609 0.117 Uiso 1 1 calc GR . . . .
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
0 1 -1 0.0817
0 -1 1 0.0523
2 -1 2 0.0807
-2 1 -2 0.1048
0 -1 0 0.0230
0 1 0 0.0145
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
O13 Mo3 Mo4 36.69(12) . . ?
O13 Mo3 O11 77.32(15) . 2_777 ?
O13 Mo3 O11 78.21(16) . . ?
O17 Mo3 Mo4 132.08(14) . . ?
O17 Mo3 O13 95.38(18) . . ?
O17 Mo3 O12 96.91(18) . . ?
O17 Mo3 O11 156.37(17) . . ?
O17 Mo3 O11 80.61(16) . 2_777 ?
O12 Mo3 Mo4 124.55(12) . . ?
O12 Mo3 O13 149.40(17) . . ?
O12 Mo3 O11 79.35(16) . . ?
O12 Mo3 O11 77.21(15) . 2_777 ?
O11 Mo3 Mo4 85.95(9) 2_777 . ?
O11 Mo3 Mo4 45.24(10) . . ?
O11 Mo3 O11 75.80(15) . 2_777 ?
O8 Mo3 Mo4 90.00(15) . . ?
O8 Mo3 O13 101.39(19) . . ?
O8 Mo3 O17 104.7(2) . . ?
O8 Mo3 O12 102.40(19) . . ?
O8 Mo3 O11 174.68(17) . 2_777 ?
O8 Mo3 O11 98.90(18) . . ?
O13 Mo4 Mo3 36.14(11) . . ?
O13 Mo4 O12 72.06(15) . 2_777 ?
O13 Mo4 O11 75.15(15) . . ?
O14 Mo4 Mo3 121.04(13) . . ?
O14 Mo4 O13 148.38(18) . . ?
O14 Mo4 O12 83.90(17) . 2_777 ?
O14 Mo4 O11 78.50(17) . . ?
O12 Mo4 Mo3 80.49(10) 2_777 . ?
O11 Mo4 Mo3 42.54(10) . . ?
O11 Mo4 O12 73.27(14) . 2_777 ?
O9 Mo4 Mo3 85.83(16) . . ?
O9 Mo4 O13 97.8(2) . . ?
O9 Mo4 O14 101.7(2) . . ?
O9 Mo4 O12 166.19(19) . 2_777 ?
O9 Mo4 O11 95.31(18) . . ?
O9 Mo4 O18 105.1(2) . . ?
O18 Mo4 Mo3 135.10(17) . . ?
O18 Mo4 O13 99.0(2) . . ?
O18 Mo4 O14 99.6(2) . . ?
O18 Mo4 O12 86.11(19) . 2_777 ?
O18 Mo4 O11 159.38(19) . . ?
O15 Mo5 O17 77.82(17) . 2_777 ?
O15 Mo5 O14 145.31(17) . . ?
O15 Mo5 O11 75.49(15) . . ?
O17 Mo5 O11 70.21(14) 2_777 . ?
O14 Mo5 O17 77.89(17) . 2_777 ?
O14 Mo5 O11 73.19(16) . . ?
O10 Mo5 O15 98.1(2) . . ?
O10 Mo5 O17 164.84(19) . 2_777 ?
O10 Mo5 O14 98.9(2) . . ?
O10 Mo5 O11 94.65(18) . . ?
O19 Mo5 O15 102.4(2) . . ?
O19 Mo5 O17 90.44(19) . 2_777 ?
O19 Mo5 O14 102.2(2) . . ?
O19 Mo5 O11 160.60(18) . . ?
O19 Mo5 O10 104.7(2) . . ?
O2 Mo1 O5 81.98(18) . . ?
O2 Mo1 N1 71.97(18) . . ?
O1 Mo1 O2 150.91(18) . . ?
O1 Mo1 O5 79.73(19) . . ?
O1 Mo1 N1 81.58(18) . . ?
O4 Mo1 O2 96.7(2) . . ?
O4 Mo1 O1 102.9(2) . . ?
O4 Mo1 O5 81.8(2) . . ?
O4 Mo1 N1 155.5(2) . . ?
N1 Mo1 O5 75.25(17) . . ?
O3 Mo1 O2 95.3(2) . . ?
O3 Mo1 O1 99.5(2) . . ?
O3 Mo1 O5 171.4(2) . . ?
O3 Mo1 O4 106.6(3) . . ?
O3 Mo1 N1 96.2(2) . . ?
O2A Mo1A O5A 77.91(16) . . ?
O2A Mo1A N1A 71.71(17) . . ?
O1A Mo1A O2A 148.36(19) . . ?
O1A Mo1A O5A 78.65(18) . . ?
O1A Mo1A N1A 82.09(18) . . ?
O4A Mo1A O2A 97.1(2) . . ?
O4A Mo1A O5A 85.2(2) . . ?
O4A Mo1A O1A 101.8(2) . . ?
O4A Mo1A N1A 159.3(2) . . ?
O4A Mo1A O3A 106.6(3) . . ?
N1A Mo1A O5A 75.60(17) . . ?
O3A Mo1A O2A 98.9(2) . . ?
O3A Mo1A O5A 168.2(2) . . ?
O3A Mo1A O1A 99.7(2) . . ?
O3A Mo1A N1A 92.6(2) . . ?
O13 Mo2 O11 71.36(13) 2_777 . ?
O15 Mo2 O13 83.66(16) . 2_777 ?
O15 Mo2 O12 145.99(17) . . ?
O15 Mo2 O11 77.37(16) . . ?
O7 Mo2 O13 162.31(18) . 2_777 ?
O7 Mo2 O15 102.5(2) . . ?
O7 Mo2 O12 95.05(19) . . ?
O7 Mo2 O11 93.62(18) . . ?
O12 Mo2 O13 71.96(15) . 2_777 ?
O12 Mo2 O11 72.63(15) . . ?
O16 Mo2 O13 89.61(19) . 2_777 ?
O16 Mo2 O15 103.0(2) . . ?
O16 Mo2 O7 104.8(2) . . ?
O16 Mo2 O12 100.3(2) . . ?
O16 Mo2 O11 160.87(18) . . ?
Mo3 O13 Mo4 107.16(18) . . ?
Mo3 O13 Mo2 112.54(17) . 2_777 ?
Mo4 O13 Mo2 104.57(17) . 2_777 ?
C8 O2 Mo1 118.8(4) . . ?
Mo2 O15 Mo5 117.3(2) . . ?
C8A O2A Mo1A 119.3(4) . . ?
Mo3 O17 Mo5 117.9(2) . 2_777 ?
C2 O1 Mo1 138.1(4) . . ?
Mo4 O14 Mo5 116.0(2) . . ?
Mo3 O12 Mo4 109.30(18) . 2_777 ?
Mo3 O12 Mo2 110.00(18) . . ?
Mo2 O12 Mo4 102.73(17) . 2_777 ?
Mo3 O11 Mo3 104.20(15) . 2_777 ?
Mo3 O11 Mo4 92.22(14) . . ?
Mo3 O11 Mo5 91.30(13) 2_777 . ?
Mo3 O11 Mo5 164.40(19) . . ?
Mo3 O11 Mo2 95.97(14) 2_777 . ?
Mo3 O11 Mo2 91.72(13) . . ?
Mo4 O11 Mo3 97.71(14) . 2_777 ?
Mo4 O11 Mo5 87.36(13) . . ?
Mo4 O11 Mo2 164.37(19) . . ?
Mo2 O11 Mo5 84.80(12) . . ?
C2A O1A Mo1A 133.8(4) . . ?
N2A N1A Mo1A 115.7(4) . . ?
C7A N1A Mo1A 128.0(4) . . ?
C7A N1A N2A 116.3(5) . . ?
C11 N3 C12 123.5(5) . . ?
N2 N1 Mo1 114.9(4) . . ?
C7 N1 Mo1 129.3(4) . . ?
C7 N1 N2 115.7(5) . . ?
C8 N2 N1 109.4(5) . . ?
C8A N2A N1A 108.4(5) . . ?
C12A N3A C11A 122.0(6) . . ?
C10 C9 C8 121.3(5) . . ?
C10 C9 C13 119.4(5) . . ?
C13 C9 C8 119.3(5) . . ?
C2 C1 C7 123.9(5) . . ?
C6 C1 C2 117.4(5) . . ?
C6 C1 C7 118.7(5) . . ?
O6A C4A C3A 116.9(5) . . ?
O6A C4A C5A 122.2(5) . . ?
C3A C4A C5A 120.8(6) . . ?
C10A C9A C8A 120.2(6) . . ?
C13A C9A C8A 121.1(5) . . ?
C13A C9A C10A 118.6(6) . . ?
O1 C2 C1 121.4(5) . . ?
O1 C2 C3 117.2(5) . . ?
C3 C2 C1 121.4(6) . . ?
O2 C8 C9 117.8(5) . . ?
N2 C8 O2 124.3(5) . . ?
N2 C8 C9 117.9(5) . . ?
C5 C6 C1 122.2(6) . . ?
C2A C3A C4A 119.7(6) . . ?
C9 C10 C11 119.7(6) . . ?
C12 C13 C9 119.3(6) . . ?
O2A C8A C9A 116.7(5) . . ?
N2A C8A O2A 124.7(6) . . ?
N2A C8A C9A 118.6(5) . . ?
C6 C5 C4 118.3(6) . . ?
O6 C4 C5 121.0(6) . . ?
O6 C4 C3 117.5(6) . . ?
C3 C4 C5 121.5(6) . . ?
N3 C12 C13 119.1(6) . . ?
N3 C11 C10 119.0(6) . . ?
C6A C1A C7A 118.7(5) . . ?
C6A C1A C2A 117.8(5) . . ?
C2A C1A C7A 123.5(5) . . ?
C5A C6A C1A 121.9(6) . . ?
N1 C7 C1 123.5(5) . . ?
N1A C7A C1A 122.9(5) . . ?
C6A C5A C4A 119.2(6) . . ?
C11A C10A C9A 118.8(7) . . ?
C2 C3 C4 119.2(6) . . ?
N3A C11A C10A 121.1(7) . . ?
O1A C2A C3A 116.3(5) . . ?
O1A C2A C1A 123.0(5) . . ?
C3A C2A C1A 120.6(5) . . ?
C12A C13A C9A 119.2(6) . . ?
N3A C12A C13A 120.3(7) . . ?
N4 C14 C15 176.9(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
Mo3 Mo4 3.1782(6) . ?
Mo3 O13 1.962(4) . ?
Mo3 O17 1.750(4) . ?
Mo3 O12 1.962(4) . ?
Mo3 O11 2.384(4) 2_777 ?
Mo3 O11 2.151(4) . ?
Mo3 O8 1.688(4) . ?
Mo4 O13 1.988(4) . ?
Mo4 O14 1.899(5) . ?
Mo4 O12 2.318(4) 2_777 ?
Mo4 O11 2.258(4) . ?
Mo4 O9 1.705(5) . ?
Mo4 O18 1.722(5) . ?
Mo5 O15 1.922(4) . ?
Mo5 O17 2.271(4) 2_777 ?
Mo5 O14 1.937(5) . ?
Mo5 O11 2.447(4) . ?
Mo5 O10 1.712(5) . ?
Mo5 O19 1.699(4) . ?
Mo1 O2 2.020(4) . ?
Mo1 O1 1.918(4) . ?
Mo1 O5 2.350(5) . ?
Mo1 O4 1.708(5) . ?
Mo1 N1 2.236(5) . ?
Mo1 O3 1.698(5) . ?
Mo1A O2A 2.004(4) . ?
Mo1A O5A 2.345(4) . ?
Mo1A O1A 1.920(4) . ?
Mo1A O4A 1.702(5) . ?
Mo1A N1A 2.241(5) . ?
Mo1A O3A 1.702(5) . ?
Mo2 O13 2.297(4) 2_777 ?
Mo2 O15 1.896(4) . ?
Mo2 O7 1.725(4) . ?
Mo2 O12 2.021(4) . ?
Mo2 O11 2.390(4) . ?
Mo2 O16 1.689(5) . ?
O2 C8 1.309(7) . ?
O2A C8A 1.321(7) . ?
O1 C2 1.348(7) . ?
O1A C2A 1.343(7) . ?
O6A C4A 1.360(7) . ?
O6 C4 1.352(7) . ?
N1A N2A 1.398(7) . ?
N1A C7A 1.296(8) . ?
N3 C12 1.351(8) . ?
N3 C11 1.331(8) . ?
N1 N2 1.399(7) . ?
N1 C7 1.287(8) . ?
N2 C8 1.294(8) . ?
N2A C8A 1.288(8) . ?
N3A C11A 1.329(10) . ?
N3A C12A 1.323(10) . ?
C9 C8 1.470(8) . ?
C9 C10 1.380(8) . ?
C9 C13 1.402(8) . ?
C1 C2 1.419(8) . ?
C1 C6 1.402(8) . ?
C1 C7 1.436(8) . ?
C4A C3A 1.396(8) . ?
C4A C5A 1.398(9) . ?
C9A C8A 1.474(8) . ?
C9A C10A 1.399(9) . ?
C9A C13A 1.393(9) . ?
C2 C3 1.376(9) . ?
C6 C5 1.381(9) . ?
C3A C2A 1.378(8) . ?
C10 C11 1.390(9) . ?
C13 C12 1.377(9) . ?
C5 C4 1.404(9) . ?
C4 C3 1.387(9) . ?
C1A C6A 1.410(8) . ?
C1A C7A 1.441(8) . ?
C1A C2A 1.419(8) . ?
C6A C5A 1.363(9) . ?
C10A C11A 1.365(9) . ?
C13A C12A 1.378(9) . ?
N4 C14 1.141(13) . ?
C14 C15 1.458(15) . ?
