#------------------------------------------------------------------------------
#$Date: 2024-06-14 04:08:29 +0300 (Fri, 14 Jun 2024) $
#$Revision: 292382 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/88/7248861.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_7248861
loop_
_publ_author_name
'Pisk, Jana'
'Vrdoljak, Višnja'
'Mandarić, Mirna'
'Hrenar, Tomica'
'Agustin, Dominique'
'Rubčić, Mirta'
_publ_section_title
;
 Impact of POM's coordination mode and Mo-hybrid constituents on the
 binding, stability, and catalytic properties of hybrid (pre)catalysts
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              19029
_journal_page_last               19040
_journal_paper_doi               10.1039/D4RA03563A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'Mo6 O19, 2(C17 H18 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C40 H48 Mo8 N6 O33'
_chemical_formula_weight         1908.36
_chemical_name_systematic
'[N'-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonium](acetone)dioxomolybdenum(vi) hexamolybdate acetone solvate'
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                104.858(2)
_cell_angle_beta                 104.620(2)
_cell_angle_gamma                94.020(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9721(3)
_cell_length_b                   10.7368(2)
_cell_length_c                   16.4964(4)
_cell_measurement_reflns_used    14257
_cell_measurement_temperature    169.99
_cell_measurement_theta_max      80.0670
_cell_measurement_theta_min      2.8910
_cell_volume                     1470.73(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      169.99
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     69.00  97.00   0.50    0.05    --   48.02  52.00  97.00   56
  2  ω    138.00 165.00   0.50    0.19    --  113.25  61.00  30.00   54
  3  ω    102.00 151.00   0.50    0.19    --  113.25  45.00   0.00   98
  4  ω    103.00 133.00   0.50    0.19    --  113.25  61.00  30.00   60
  5  ω     99.00 175.00   0.50    0.19    --  113.25  61.00  60.00  152
  6  ω    114.00 178.00   0.50    0.19    --  113.25  52.00  97.00  128
  7  ω    126.00 175.00   0.50    0.19    --  113.25  45.00 120.00   98
  8  ω    142.00 172.00   0.50    0.19    --  113.25  30.00 150.00   60
  9  ω    101.00 149.00   0.50    0.19    --  113.25  45.00  90.00   96
 10  ω    114.00 158.00   0.50    0.19    --  113.25  30.00   0.00   88
 11  ω    113.00 144.00   0.50    0.19    --  113.25  30.00 -90.00   62
 12  ω    138.00 172.00   0.50    0.19    --  113.25  45.00-150.00   68
 13  ω    144.00 173.00   0.50    0.19    --  113.25  15.00-150.00   58
 14  ω    115.00 141.00   0.50    0.19    --  113.25  15.00-150.00   52
 15  ω    -20.00  25.00   0.50    0.05    --   48.02 -19.00-150.00   90
 16  ω    -21.00  59.00   0.50    0.05    --   48.02 -52.00 -47.00  160
 17  ω    -12.00  63.00   0.50    0.05    --   48.02 -57.00  90.00  150
 18  ω     42.00 109.00   0.50    0.19    --  113.25-125.00  60.00  134
 19  ω     93.00 118.00   0.50    0.19    --  113.25-134.00   1.06   50
 20  ω     46.00  72.00   0.50    0.19    --  113.25-134.00   1.06   52
 21  ω     85.00 111.00   0.50    0.19    --  113.25-125.00 -90.00   52
 22  ω     62.00 111.00   0.50    0.19    --  113.25-125.00-150.00   98
 23  ω     43.00  78.00   0.50    0.19    --  113.25-125.00-180.00   70
 24  ω     84.00 111.00   0.50    0.19    --  113.25-125.00-180.00   54
 25  ω     35.00  96.00   0.50    0.05    --   48.02-125.00 -30.00  122
 26  ω     69.00 110.00   0.50    0.19    --  113.25-125.00  90.00   82
 27  ω     84.00 110.00   0.50    0.19    --  113.25-125.00 150.00   52
 28  ω     45.00 104.00   0.50    0.19    --  113.25 -95.00  60.00  118
 29  ω     64.00 108.00   0.50    0.19    --  113.25-110.00  18.97   88
 30  ω     77.00 102.00   0.50    0.19    --  113.25 -95.00   0.00   50
 31  ω     42.00  69.00   0.50    0.19    --  113.25-108.00-100.20   54
 32  ω     45.00  79.00   0.50    0.19    --  113.25 -99.00-150.56   68
 33  ω     80.00 107.00   0.50    0.19    --  113.25-108.00-100.20   54
 34  ω     71.00 102.00   0.50    0.19    --  113.25 -95.00 -90.00   62
 35  ω     54.00 104.00   0.50    0.19    --  113.25 -95.00 -60.00  100
 36  ω     43.00  96.00   0.50    0.19    --  113.25 -95.00  90.00  106
 37  ω     46.00  71.00   0.50    0.19    --  113.25 -61.00  90.00   50
 38  ω     56.00  88.00   0.50    0.19    --  113.25 -77.00  90.00   64
 39  ω     73.00 101.00   0.50    0.19    --  113.25 -77.00 -60.00   56
 40  ω     44.00  69.00   0.50    0.19    --  113.25 -77.00 -60.00   50
 41  ω     43.00  69.00   0.50    0.19    --  113.25 -61.00 -60.00   52
 42  ω     44.00  70.00   0.50    0.19    --  113.25 -77.00-120.00   52
 43  ω     45.00  70.00   0.50    0.19    --  113.25 -61.00-120.00   50
 44  ω     42.00  68.00   0.50    0.19    --  113.25 -61.00 -90.00   52
 45  ω     42.00  68.00   0.50    0.19    --  113.25 -61.00 150.00   52
 46  ω    114.00 167.00   0.50    0.19    --  113.25 125.00 -90.00  106
 47  ω     96.00 140.00   0.50    0.19    --  113.25 125.00 -30.00   88
 48  ω    150.00 176.00   0.50    0.19    --  113.25 125.00 -30.00   52
 49  ω    -20.00  23.00   0.50    0.05    --  -48.02  52.00  97.00   86
 50  ω    -53.00 -23.00   0.50    0.05    --  -48.02  52.00  97.00   60
 51  ω    -56.00 -31.00   0.50    0.19    --  -91.75  52.00  97.00   50
 52  ω    -70.00 -22.00   0.50    0.19    --  -91.75  61.00 -90.00   96
 53  ω    -46.00 -21.00   0.50    0.19    --  -91.75  45.00-120.00   50
 54  ω    -51.00 -21.00   0.50    0.19    --  -91.75  45.00-150.00   60
 55  ω   -118.00 -65.00   0.50    0.05    --  -48.02 -52.00 -47.00  106
 56  ω   -120.00 -95.00   0.50    0.05    --  -48.02-125.00 -60.00   50
 57  ω   -119.00 -81.00   0.50    0.05    --  -48.02-125.00-120.00   76
 58  ω   -121.00 -96.00   0.50    0.19    --  -91.75 -52.00 -47.00   50
 59  ω   -111.00 -76.00   0.50    0.05    --  -48.02-125.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0846773000
_diffrn_orient_matrix_UB_12      0.0515922000
_diffrn_orient_matrix_UB_13      -0.0578610000
_diffrn_orient_matrix_UB_21      -0.1360409000
_diffrn_orient_matrix_UB_22      0.0743879000
_diffrn_orient_matrix_UB_23      -0.0272258000
_diffrn_orient_matrix_UB_31      0.0804999000
_diffrn_orient_matrix_UB_32      0.1196205000
_diffrn_orient_matrix_UB_33      0.0777350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18183
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.522
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.194
_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    2.155
_exptl_crystal_description       plate
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.389
_refine_diff_density_min         -2.465
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00063(9)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0647P)²+5.8824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5659
_reflns_number_total             6056
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           1Ha-2CH3COCH3
_cod_database_code               7248861
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo4 O17 C18 N3'
_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   0.972
_shelx_estimated_absorpt_t_min   0.157
_diffrn_oxdiff_digest_frames
;
017a254803ed035e4dbb6c008c31acfcde04474c95e
;
_diffrn_oxdiff_digest_hkl
;
011e8965894199009e7d02648f50bc13e049c5
;
_reflns_odcompleteness_completeness 96.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5)
 Fixed Uiso: H3(0.029) H7(0.028) H10(0.029) H6(0.032) H13(0.03) H11(0.033)
 H4(0.044) H5(0.04) H12(0.034) H16A(0.065) H16B(0.065) H16C(0.065) H17A(0.049)
 H17B(0.049) H17C(0.049) H20A(0.085) H20B(0.085) H20C(0.085) H14A(0.103)
 H14B(0.103) H14C(0.103) H21A(0.074) H21B(0.074) H21C(0.074) H19A(0.131)
 H19B(0.131) H19C(0.131)
 Fixed X: O11(0) H3(0.558754) H7(0.229358) H10(0.458911) H6(0.10687)
 H13(0.548532) H11(0.651168) H4(-0.008301) H5(-0.004699) H12(0.645205)
 H16A(0.306313) H16B(0.165058) H16C(0.18645) H17A(-0.119318) H17B(-0.075916)
 H17C(-0.123387) H20A(0.438) H20B(0.479433) H20C(0.615203) H14A(-0.068009)
 H14B(0.099195) H14C(0.052487) H21A(0.293833) H21B(0.236462) H21C(0.291663)
 H19A(0.614686) H19B(0.430426) H19C(0.525722)
 Fixed Y: O11(0.5) H3(0.859616) H7(1.037632) H10(0.907202) H6(1.175552)
 H13(0.55662) H11(0.676219) H4(1.067475) H5(1.216396) H12(0.516605)
 H16A(0.453075) H16B(0.358838) H16C(0.360837) H17A(0.411712) H17B(0.463517)
 H17C(0.561314) H20A(1.269152) H20B(1.266134) H20C(1.274673) H14A(0.872545)
 H14B(0.94226) H14C(0.788361) H21A(0.948473) H21B(1.072127) H21C(1.079801)
 H19A(1.098304) H19B(1.065962) H19C(0.956217)
 Fixed Z: O11(0) H3(0.182985) H7(0.480085) H10(0.296871) H6(0.574798)
 H13(0.3314) H11(0.13596) H4(0.770846) H5(0.689281) H12(0.208366)
 H16A(0.415659) H16B(0.340031) H16C(0.43967) H17A(0.370518) H17B(0.295446)
 H17C(0.372769) H20A(0.208933) H20B(0.119671) H20C(0.205973) H14A(0.799923)
 H14B(0.863792) H14C(0.842625) H21A(0.130374) H21B(0.10105) H21C(0.202561)
 H19A(0.05337) H19B(0.009922) H19C(0.03832)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.603
_oxdiff_exptl_absorpt_empirical_full_min 0.639
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
Mo2 Mo 0.08980(4) 0.54764(4) 0.15044(2) 0.02275(13) Uani 1 1 d . . . . .
Mo1 Mo 0.38980(4) 0.73595(4) 0.56472(2) 0.02181(13) Uani 1 1 d . . . . .
Mo3 Mo 0.23090(5) 0.60779(5) -0.00219(3) 0.03574(15) Uani 1 1 d . . . . .
Mo4 Mo 0.10565(6) 0.30759(5) -0.01413(3) 0.03827(15) Uani 1 1 d . . . . .
O11 O 0.000000 0.500000 0.000000 0.0181(9) Uani 1 2 d S T P . .
O2 O 0.4545(4) 0.6899(3) 0.4536(2) 0.0239(7) Uani 1 1 d . . . . .
O1 O 0.2376(5) 0.8018(4) 0.6216(2) 0.0315(8) Uani 1 1 d . . . . .
O4 O 0.4031(4) 0.5912(4) 0.5876(2) 0.0289(8) Uani 1 1 d . . . . .
O9 O 0.1587(5) 0.3845(4) 0.1113(2) 0.0340(9) Uani 1 1 d . . . . .
O6 O 0.1479(4) 0.6286(3) 0.4603(2) 0.0254(7) Uani 1 1 d . . . . .
O12 O 0.1161(5) 0.5498(5) -0.1233(3) 0.0409(10) Uani 1 1 d . . . . .
O8 O 0.1538(5) 0.5850(4) 0.2601(2) 0.0339(9) Uani 1 1 d . . . . .
O10 O 0.2549(5) 0.6295(4) 0.1211(2) 0.0368(9) Uani 1 1 d . . . . .
O15 O 0.0203(6) 0.3087(5) -0.1329(3) 0.0459(11) Uani 1 1 d . . . . .
N3 N 0.5561(5) 0.8010(4) 0.2116(3) 0.0242(8) Uani 1 1 d . . . . .
H3 H 0.558754 0.859616 0.182985 0.029 Uiso 1 1 calc R . . . .
O14 O 0.2753(5) 0.4368(6) -0.0109(3) 0.0475(12) Uani 1 1 d . . . . .
O5 O 0.1044(7) 0.8426(4) 0.7462(3) 0.0470(12) Uani 1 1 d . . . . .
N2 N 0.3596(5) 0.8692(4) 0.4161(3) 0.0218(8) Uani 1 1 d . . . . .
N1 N 0.3130(5) 0.8798(4) 0.4914(2) 0.0208(8) Uani 1 1 d . . . . .
O3 O 0.5531(5) 0.8372(4) 0.6310(3) 0.0397(10) Uani 1 1 d . . . . .
O17 O -0.0969(6) 0.2561(4) -0.0099(3) 0.0462(11) Uani 1 1 d . . . . .
C1 C 0.1761(6) 0.9999(5) 0.5872(3) 0.0237(9) Uani 1 1 d . . . . .
C7 C 0.2406(6) 0.9775(5) 0.5138(3) 0.0231(9) Uani 1 1 d . . . . .
H7 H 0.229358 1.037632 0.480085 0.028 Uiso 1 1 calc R . . . .
C10 C 0.4974(6) 0.8271(5) 0.2801(3) 0.0239(9) Uani 1 1 d . . . . .
H10 H 0.458911 0.907202 0.296871 0.029 Uiso 1 1 calc R . . . .
C9 C 0.4932(5) 0.7368(5) 0.3264(3) 0.0207(9) Uani 1 1 d . . . . .
C8 C 0.4321(5) 0.7674(5) 0.4035(3) 0.0194(8) Uani 1 1 d . . . . .
C6 C 0.1068(6) 1.1151(5) 0.6080(3) 0.0265(10) Uani 1 1 d . . . . .
H6 H 0.106870 1.175552 0.574798 0.032 Uiso 1 1 calc R . . . .
C13 C 0.5497(6) 0.6197(5) 0.3003(3) 0.0248(10) Uani 1 1 d . . . . .
H13 H 0.548532 0.556620 0.331400 0.030 Uiso 1 1 calc R . . . .
C2 C 0.1756(6) 0.9121(5) 0.6367(3) 0.0252(10) Uani 1 1 d . . . . .
O13 O 0.3977(6) 0.6926(8) -0.0003(3) 0.072(2) Uani 1 1 d . . . . .
C11 C 0.6104(6) 0.6905(5) 0.1849(3) 0.0277(10) Uani 1 1 d . . . . .
H11 H 0.651168 0.676219 0.135960 0.033 Uiso 1 1 calc R . . . .
C4 C 0.0383(7) 1.0502(6) 0.7242(4) 0.0365(13) Uani 1 1 d . . . . .
H4 H -0.008301 1.067475 0.770846 0.044 Uiso 1 1 calc R . . . .
C5 C 0.0403(6) 1.1390(5) 0.6754(4) 0.0335(12) Uani 1 1 d . . . . .
H5 H -0.004699 1.216396 0.689281 0.040 Uiso 1 1 calc R . . . .
C12 C 0.6078(6) 0.5964(5) 0.2278(3) 0.0285(10) Uani 1 1 d . . . . .
H12 H 0.645205 0.516605 0.208366 0.034 Uiso 1 1 calc R . . . .
C3 C 0.1036(7) 0.9373(6) 0.7048(4) 0.0330(11) Uani 1 1 d . . . . .
C15 C 0.0978(6) 0.5184(5) 0.4107(3) 0.0242(9) Uani 1 1 d . . . . .
O16 O 0.1903(9) 0.1718(6) -0.0252(4) 0.083(2) Uani 1 1 d . . . . .
O7 O 0.5489(12) 1.0254(6) 0.1733(4) 0.107(3) Uani 1 1 d . . . . .
C16 C 0.1974(8) 0.4139(6) 0.4007(5) 0.0432(15) Uani 1 1 d . . . . .
H16A H 0.306313 0.453075 0.415659 0.065 Uiso 1 1 calc GR . . . .
H16B H 0.165058 0.358838 0.340031 0.065 Uiso 1 1 calc GR . . . .
H16C H 0.186450 0.360837 0.439670 0.065 Uiso 1 1 calc GR . . . .
C17 C -0.0697(6) 0.4859(6) 0.3578(4) 0.0327(11) Uani 1 1 d . . . . .
H17A H -0.119318 0.411712 0.370518 0.049 Uiso 1 1 calc GR . . . .
H17B H -0.075916 0.463517 0.295446 0.049 Uiso 1 1 calc GR . . . .
H17C H -0.123387 0.561314 0.372769 0.049 Uiso 1 1 calc GR . . . .
C20 C 0.5071(12) 1.2382(7) 0.1730(5) 0.057(2) Uani 1 1 d . . . . .
H20A H 0.438000 1.269152 0.208933 0.085 Uiso 1 1 calc GR . . . .
H20B H 0.479433 1.266134 0.119671 0.085 Uiso 1 1 calc GR . . . .
H20C H 0.615203 1.274673 0.205973 0.085 Uiso 1 1 calc GR . . . .
C18 C 0.4905(10) 1.0961(7) 0.1497(5) 0.065(3) Uani 1 1 d D . . . .
C14 C 0.0422(14) 0.8630(8) 0.8187(5) 0.068(3) Uani 1 1 d . . . . .
H14A H -0.068009 0.872545 0.799923 0.103 Uiso 1 1 calc GR . . . .
H14B H 0.099195 0.942260 0.863792 0.103 Uiso 1 1 calc GR . . . .
H14C H 0.052487 0.788361 0.842625 0.103 Uiso 1 1 calc GR . . . .
C21 C 0.3096(16) 1.0438(17) 0.1455(9) 0.050(3) Uani 0.5 1 d . . . A .
H21A H 0.293833 0.948473 0.130374 0.074 Uiso 0.5 1 calc GR . . . .
H21B H 0.236462 1.072127 0.101050 0.074 Uiso 0.5 1 calc GR . . . .
H21C H 0.291663 1.079801 0.202561 0.074 Uiso 0.5 1 calc GR . . . .
C19 C 0.518(3) 1.050(2) 0.0532(12) 0.087(8) Uani 0.5 1 d D . . A -1
H19A H 0.614686 1.098304 0.053370 0.131 Uiso 0.5 1 calc GR . . A -1
H19B H 0.430426 1.065962 0.009922 0.131 Uiso 0.5 1 calc GR . . A -1
H19C H 0.525722 0.956217 0.038320 0.131 Uiso 0.5 1 calc GR . . A -1
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
-5 0 7 0.0361
5 0 -7 0.0494
1 4 5 0.0836
-1 -4 -6 0.1027
0 -6 6 0.0010
0 6 -6 0.0010
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
O9 Mo2 O11 77.16(11) . . ?
O9 Mo2 O12 87.0(2) . 2_565 ?
O9 Mo2 O15 153.62(17) . 2_565 ?
O12 Mo2 O11 76.67(11) 2_565 . ?
O8 Mo2 O11 178.90(16) . . ?
O8 Mo2 O9 103.95(19) . . ?
O8 Mo2 O12 103.37(18) . 2_565 ?
O8 Mo2 O10 102.91(18) . . ?
O8 Mo2 O15 102.4(2) . 2_565 ?
O10 Mo2 O11 77.00(11) . . ?
O10 Mo2 O9 88.8(2) . . ?
O10 Mo2 O12 153.63(16) . 2_565 ?
O10 Mo2 O15 87.3(2) . 2_565 ?
O15 Mo2 O11 76.53(12) 2_565 . ?
O15 Mo2 O12 85.1(2) 2_565 2_565 ?
O2 Mo1 O6 78.92(13) . . ?
O2 Mo1 N1 71.93(14) . . ?
O1 Mo1 O2 147.39(15) . . ?
O1 Mo1 O6 76.96(15) . . ?
O1 Mo1 N1 80.98(15) . . ?
O4 Mo1 O2 97.92(16) . . ?
O4 Mo1 O1 101.58(17) . . ?
O4 Mo1 O6 85.22(16) . . ?
O4 Mo1 N1 159.55(17) . . ?
O4 Mo1 O3 106.0(2) . . ?
N1 Mo1 O6 75.53(13) . . ?
O3 Mo1 O2 98.68(19) . . ?
O3 Mo1 O1 100.7(2) . . ?
O3 Mo1 O6 168.75(17) . . ?
O3 Mo1 N1 93.25(18) . . ?
O12 Mo3 O11 77.17(12) . . ?
O12 Mo3 O10 153.30(16) . . ?
O12 Mo3 O17 86.8(2) . 2_565 ?
O10 Mo3 O11 76.19(11) . . ?
O10 Mo3 O17 85.2(2) . 2_565 ?
O14 Mo3 O11 77.33(14) . . ?
O14 Mo3 O12 88.3(2) . . ?
O14 Mo3 O10 87.5(2) . . ?
O14 Mo3 O17 153.5(2) . 2_565 ?
O17 Mo3 O11 76.20(13) 2_565 . ?
O13 Mo3 O11 177.2(3) . . ?
O13 Mo3 O12 104.4(2) . . ?
O13 Mo3 O10 102.1(2) . . ?
O13 Mo3 O14 104.9(3) . . ?
O13 Mo3 O17 101.6(3) . 2_565 ?
O9 Mo4 O11 76.54(11) . . ?
O9 Mo4 O14 85.53(18) . . ?
O15 Mo4 O11 76.73(13) . . ?
O15 Mo4 O9 153.17(17) . . ?
O15 Mo4 O14 85.7(2) . . ?
O14 Mo4 O11 75.76(13) . . ?
O17 Mo4 O11 77.53(14) . . ?
O17 Mo4 O9 87.39(19) . . ?
O17 Mo4 O15 89.1(2) . . ?
O17 Mo4 O14 153.3(2) . . ?
O16 Mo4 O11 177.1(3) . . ?
O16 Mo4 O9 103.8(2) . . ?
O16 Mo4 O15 102.7(2) . . ?
O16 Mo4 O14 101.3(3) . . ?
O16 Mo4 O17 105.4(4) . . ?
Mo2 O11 Mo2 180.0 . 2_565 ?
Mo2 O11 Mo3 89.898(14) 2_565 2_565 ?
Mo2 O11 Mo3 90.102(14) 2_565 . ?
Mo2 O11 Mo3 89.897(14) . . ?
Mo2 O11 Mo3 90.103(14) . 2_565 ?
Mo2 O11 Mo4 89.892(15) 2_565 2_565 ?
Mo2 O11 Mo4 89.893(15) . . ?
Mo2 O11 Mo4 90.108(15) . 2_565 ?
Mo2 O11 Mo4 90.108(15) 2_565 . ?
Mo3 O11 Mo3 180.0 2_565 . ?
Mo3 O11 Mo4 89.84(2) 2_565 . ?
Mo3 O11 Mo4 89.84(2) . 2_565 ?
Mo3 O11 Mo4 90.16(2) . . ?
Mo3 O11 Mo4 90.16(2) 2_565 2_565 ?
Mo4 O11 Mo4 180.0 . 2_565 ?
C8 O2 Mo1 118.6(3) . . ?
C2 O1 Mo1 136.4(3) . . ?
Mo2 O9 Mo4 116.41(19) . . ?
C15 O6 Mo1 136.0(3) . . ?
Mo3 O12 Mo2 116.06(19) . 2_565 ?
Mo2 O10 Mo3 116.84(19) . . ?
Mo4 O15 Mo2 116.5(2) . 2_565 ?
C10 N3 H3 118.6 . . ?
C11 N3 H3 118.6 . . ?
C11 N3 C10 122.8(4) . . ?
Mo3 O14 Mo4 116.7(2) . . ?
C3 O5 C14 118.4(6) . . ?
C8 N2 N1 108.1(4) . . ?
N2 N1 Mo1 115.9(3) . . ?
C7 N1 Mo1 128.1(3) . . ?
C7 N1 N2 115.8(4) . . ?
Mo4 O17 Mo3 116.4(2) . 2_565 ?
C6 C1 C7 118.1(5) . . ?
C2 C1 C7 122.6(4) . . ?
C2 C1 C6 119.3(5) . . ?
N1 C7 C1 123.6(5) . . ?
N1 C7 H7 118.2 . . ?
C1 C7 H7 118.2 . . ?
N3 C10 H10 120.2 . . ?
N3 C10 C9 119.6(5) . . ?
C9 C10 H10 120.2 . . ?
C10 C9 C8 119.4(4) . . ?
C10 C9 C13 119.1(4) . . ?
C13 C9 C8 121.4(4) . . ?
O2 C8 N2 125.1(4) . . ?
O2 C8 C9 117.1(4) . . ?
N2 C8 C9 117.8(4) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.3(5) . . ?
C5 C6 H6 119.9 . . ?
C9 C13 H13 120.4 . . ?
C12 C13 C9 119.2(5) . . ?
C12 C13 H13 120.4 . . ?
O1 C2 C1 123.2(4) . . ?
O1 C2 C3 117.3(5) . . ?
C1 C2 C3 119.5(5) . . ?
N3 C11 H11 119.9 . . ?
N3 C11 C12 120.3(5) . . ?
C12 C11 H11 119.9 . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.4(5) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C13 C12 H12 120.4 . . ?
C11 C12 C13 119.1(5) . . ?
C11 C12 H12 120.4 . . ?
O5 C3 C2 114.5(5) . . ?
O5 C3 C4 125.4(5) . . ?
C4 C3 C2 120.2(6) . . ?
O6 C15 C16 122.5(5) . . ?
O6 C15 C17 119.8(5) . . ?
C16 C15 C17 117.7(5) . . ?
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 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
O7 C18 C20 136.9(8) . . ?
O7 C18 C21 100.1(11) . . ?
O7 C18 C19 95.1(11) . . ?
C20 C18 C21 106.9(9) . . ?
C20 C18 C19 105.9(10) . . ?
C19 C18 C21 110.4(12) . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
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
Mo2 O11 2.3134(4) . ?
Mo2 O9 1.908(4) . ?
Mo2 O12 1.944(4) 2_565 ?
Mo2 O8 1.683(4) . ?
Mo2 O10 1.897(4) . ?
Mo2 O15 1.933(4) 2_565 ?
Mo1 O2 2.014(3) . ?
Mo1 O1 1.920(4) . ?
Mo1 O4 1.696(4) . ?
Mo1 O6 2.398(4) . ?
Mo1 N1 2.238(4) . ?
Mo1 O3 1.697(4) . ?
Mo3 O11 2.3142(4) . ?
Mo3 O12 1.916(4) . ?
Mo3 O10 1.940(4) . ?
Mo3 O14 1.883(5) . ?
Mo3 O17 1.959(5) 2_565 ?
Mo3 O13 1.686(5) . ?
Mo4 O11 2.3152(4) . ?
Mo4 O9 1.939(4) . ?
Mo4 O15 1.920(4) . ?
Mo4 O14 1.967(6) . ?
Mo4 O17 1.886(5) . ?
Mo4 O16 1.681(5) . ?
O2 C8 1.307(6) . ?
O1 C2 1.336(6) . ?
O6 C15 1.231(6) . ?
N3 H3 0.8800 . ?
N3 C10 1.339(6) . ?
N3 C11 1.327(7) . ?
O5 C3 1.362(8) . ?
O5 C14 1.418(8) . ?
N2 N1 1.389(5) . ?
N2 C8 1.309(6) . ?
N1 C7 1.294(6) . ?
C1 C7 1.443(7) . ?
C1 C6 1.425(7) . ?
C1 C2 1.397(7) . ?
C7 H7 0.9500 . ?
C10 H10 0.9500 . ?
C10 C9 1.384(7) . ?
C9 C8 1.478(7) . ?
C9 C13 1.395(7) . ?
C6 H6 0.9500 . ?
C6 C5 1.368(8) . ?
C13 H13 0.9500 . ?
C13 C12 1.393(7) . ?
C2 C3 1.410(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.377(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.398(9) . ?
C4 C3 1.381(8) . ?
C5 H5 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.484(7) . ?
C15 C17 1.501(7) . ?
O7 C18 1.053(10) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C18 1.461(10) . ?
C18 C21 1.658(17) . ?
C18 C19 1.629(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
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
Mo1 O2 C8 N2 -5.4(6) . . . . ?
Mo1 O2 C8 C9 174.9(3) . . . . ?
Mo1 O1 C2 C1 21.6(8) . . . . ?
Mo1 O1 C2 C3 -160.0(4) . . . . ?
Mo1 O6 C15 C16 -4.1(8) . . . . ?
Mo1 O6 C15 C17 175.9(3) . . . . ?
Mo1 N1 C7 C1 -9.2(7) . . . . ?
O11 Mo2 O10 Mo3 -2.3(2) . . . . ?
O11 Mo3 O14 Mo4 1.34(18) . . . . ?
O11 Mo4 O17 Mo3 0.00(18) . . . 2_565 ?
O1 C2 C3 O5 -1.1(8) . . . . ?
O1 C2 C3 C4 179.5(5) . . . . ?
O9 Mo2 O10 Mo3 74.8(3) . . . . ?
O9 Mo4 O17 Mo3 76.8(2) . . . 2_565 ?
O12 Mo2 O10 Mo3 -5.9(6) 2_565 . . . ?
O12 Mo3 O14 Mo4 -75.9(2) . . . . ?
O8 Mo2 O10 Mo3 178.8(3) . . . . ?
O10 Mo3 O14 Mo4 77.7(2) . . . . ?
O15 Mo2 O10 Mo3 -79.1(3) 2_565 . . . ?
O15 Mo4 O17 Mo3 -76.6(3) . . . 2_565 ?
N3 C10 C9 C8 178.4(4) . . . . ?
N3 C10 C9 C13 -0.3(7) . . . . ?
N3 C11 C12 C13 -0.9(8) . . . . ?
O14 Mo4 O17 Mo3 2.1(6) . . . 2_565 ?
N2 N1 C7 C1 176.4(4) . . . . ?
N1 N2 C8 O2 0.5(6) . . . . ?
N1 N2 C8 C9 -179.8(4) . . . . ?
O17 Mo3 O14 Mo4 3.6(6) 2_565 . . . ?
C1 C6 C5 C4 -0.6(8) . . . . ?
C1 C2 C3 O5 177.4(5) . . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C7 C1 C6 C5 178.2(5) . . . . ?
C7 C1 C2 O1 1.5(8) . . . . ?
C7 C1 C2 C3 -176.9(5) . . . . ?
C10 N3 C11 C12 0.1(8) . . . . ?
C10 C9 C8 O2 -168.7(4) . . . . ?
C10 C9 C8 N2 11.6(6) . . . . ?
C10 C9 C13 C12 -0.4(7) . . . . ?
C9 C13 C12 C11 1.1(8) . . . . ?
C8 N2 N1 Mo1 4.1(5) . . . . ?
C8 N2 N1 C7 179.2(4) . . . . ?
C8 C9 C13 C12 -179.2(4) . . . . ?
C6 C1 C7 N1 176.5(5) . . . . ?
C6 C1 C2 O1 179.9(5) . . . . ?
C6 C1 C2 C3 1.5(7) . . . . ?
C13 C9 C8 O2 10.0(7) . . . . ?
C13 C9 C8 N2 -169.7(4) . . . . ?
C2 C1 C7 N1 -5.1(8) . . . . ?
C2 C1 C6 C5 -0.2(7) . . . . ?
O13 Mo3 O14 Mo4 179.6(2) . . . . ?
C11 N3 C10 C9 0.5(7) . . . . ?
C5 C4 C3 O5 -178.1(6) . . . . ?
C5 C4 C3 C2 1.2(9) . . . . ?
C3 C4 C5 C6 0.1(9) . . . . ?
O16 Mo4 O17 Mo3 -179.6(3) . . . 2_565 ?
C14 O5 C3 C2 176.6(7) . . . . ?
C14 O5 C3 C4 -4.1(10) . . . . ?
loop_
_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
-5.3380 -0.3472 6.6207 -0.8530 0.5201 0.0434
5.3574 0.4048 -6.5477 0.8534 -0.5204 -0.0293
1.1271 4.0580 5.4518 -0.0106 0.0001 0.9999
-0.9263 -4.0344 -5.6828 0.0422 -0.0194 -0.9989
0.3745 -6.4506 6.3043 -0.6659 -0.7024 -0.2514
-0.3745 6.4506 -6.3043 0.6659 0.7024 0.2514
