# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_importp
_database_code_depnum_ccdc_archive 'CCDC 919555'
#TrackingRef 'Master_archive.cif'
_audit_creation_date             2012-07-05T18:16:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Chisholm 1904'
_chemical_formula_moiety         'C84 H80 Mo2 N4 O8 S2, 2(C4 H8 O)'
_chemical_formula_sum            'C92 H96 Mo2 N4 O10 S2'
_chemical_formula_weight         1673.73
_chemical_compound_source        'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   12.6203(2)
_cell_length_b                   13.1151(2)
_cell_length_c                   13.4075(2)
_cell_angle_alpha                81.3950(10)
_cell_angle_beta                 89.3820(10)
_cell_angle_gamma                84.0390(10)
_cell_volume                     2182.29(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7670
_cell_measurement_theta_min      1.018
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_special_details           
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.9433
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.767793E-1
_diffrn_orient_matrix_ub_12      -0.76053E-2
_diffrn_orient_matrix_ub_13      -0.195719E-1
_diffrn_orient_matrix_ub_21      -0.58992E-2
_diffrn_orient_matrix_ub_22      0.748025E-1
_diffrn_orient_matrix_ub_23      -0.30408E-1
_diffrn_orient_matrix_ub_31      0.20428E-1
_diffrn_orient_matrix_ub_32      0.189184E-1
_diffrn_orient_matrix_ub_33      0.662024E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     ?
_diffrn_reflns_number            14970
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             7685
_reflns_number_gt                6377
_reflns_threshold_expression     >2\s(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
One of the isopropyls was disordered over two locations the two parts were
restrained using the SAME command. The methine carbon (C34) was used as the
pivot point and C34A/C34B were held together using the EXYZ and
EADP constraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.3378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7685
_refine_ls_number_parameters     515
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.085
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.08
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42754(19) 0.62326(18) 0.63731(17) 0.0298(5) Uani 1 1 d . . .
C2 C 0.3943(2) 0.68472(19) 0.71778(18) 0.0335(6) Uani 1 1 d . . .
C3 C 0.3126(2) 0.6468(2) 0.7842(2) 0.0406(6) Uani 1 1 d . . .
C4 C 0.4406(2) 0.77078(19) 0.72908(18) 0.0347(6) Uani 1 1 d . . .
H4 H 0.4941 0.7876 0.6808 0.042 Uiso 1 1 calc R . .
C5 C 0.4230(2) 0.84073(19) 0.80104(19) 0.0365(6) Uani 1 1 d . . .
C6 C 0.4747(2) 0.9273(2) 0.8043(2) 0.0413(6) Uani 1 1 d . . .
H6 H 0.5289 0.9472 0.7579 0.05 Uiso 1 1 calc R . .
C7 C 0.4413(2) 0.9835(2) 0.8810(2) 0.0407(6) Uani 1 1 d . . .
H7 H 0.4698 1.0453 0.8916 0.049 Uiso 1 1 calc R . .
C8 C 0.3632(2) 0.94071(19) 0.93974(19) 0.0353(6) Uani 1 1 d . . .
C9 C 0.3059(2) 0.97668(19) 1.02538(19) 0.0356(6) Uani 1 1 d . . .
C10 C 0.2579(2) 0.9085(2) 1.09744(19) 0.0406(6) Uani 1 1 d . . .
H10 H 0.269 0.8361 1.0949 0.049 Uiso 1 1 calc R . .
C11 C 0.1947(2) 0.9436(2) 1.1723(2) 0.0418(6) Uani 1 1 d . . .
H11 H 0.1632 0.8952 1.2204 0.05 Uiso 1 1 calc R . .
C12 C 0.1764(2) 1.04920(19) 1.17858(19) 0.0366(6) Uani 1 1 d . . .
C13 C 0.2312(2) 1.1172(2) 1.11178(19) 0.0389(6) Uani 1 1 d . . .
H13 H 0.2251 1.1888 1.1179 0.047 Uiso 1 1 calc R . .
C14 C 0.2943(2) 1.0812(2) 1.03688(19) 0.0383(6) Uani 1 1 d . . .
H14 H 0.3306 1.1289 0.9921 0.046 Uiso 1 1 calc R . .
C15 C 0.0077(2) 1.03921(19) 1.2726(2) 0.0386(6) Uani 1 1 d . . .
C16 C -0.0373(2) 1.0439(2) 1.3669(2) 0.0511(7) Uani 1 1 d . . .
H16 H -0.0024 1.0752 1.415 0.061 Uiso 1 1 calc R . .
C17 C -0.1334(3) 1.0029(2) 1.3914(3) 0.0625(9) Uani 1 1 d . . .
H17 H -0.1642 1.0072 1.4558 0.075 Uiso 1 1 calc R . .
C18 C -0.1839(2) 0.9562(2) 1.3225(3) 0.0613(9) Uani 1 1 d . . .
H18 H -0.2489 0.9274 1.3394 0.074 Uiso 1 1 calc R . .
C19 C -0.1394(2) 0.9517(2) 1.2294(2) 0.0523(8) Uani 1 1 d . . .
H19 H -0.1742 0.9196 1.1817 0.063 Uiso 1 1 calc R . .
C20 C -0.0456(2) 0.9928(2) 1.2039(2) 0.0445(7) Uani 1 1 d . . .
H20 H -0.0166 0.9895 1.1387 0.053 Uiso 1 1 calc R . .
C21 C 0.1130(2) 1.1851(2) 1.27854(19) 0.0403(6) Uani 1 1 d . . .
C22 C 0.0336(3) 1.2651(2) 1.2547(2) 0.0491(7) Uani 1 1 d . . .
H22 H -0.0292 1.2544 1.2209 0.059 Uiso 1 1 calc R . .
C23 C 0.0468(3) 1.3624(2) 1.2811(2) 0.0644(10) Uani 1 1 d . . .
H23 H -0.0065 1.4189 1.2642 0.077 Uiso 1 1 calc R . .
C24 C 0.1375(3) 1.3754(3) 1.3316(3) 0.0695(10) Uani 1 1 d . . .
H24 H 0.146 1.4412 1.3502 0.083 Uiso 1 1 calc R . .
C25 C 0.2148(3) 1.2966(3) 1.3552(3) 0.0704(10) Uani 1 1 d . . .
H25 H 0.2768 1.3071 1.3902 0.084 Uiso 1 1 calc R . .
C26 C 0.2038(3) 1.2006(3) 1.3285(2) 0.0551(8) Uani 1 1 d . . .
H26 H 0.2585 1.1452 1.3445 0.066 Uiso 1 1 calc R . .
C27 C 0.34060(19) 0.57529(18) 0.36588(17) 0.0290(5) Uani 1 1 d . . .
C28 C 0.25367(19) 0.61307(18) 0.29032(17) 0.0298(5) Uani 1 1 d . A .
C29 C 0.26348(19) 0.58539(19) 0.19327(18) 0.0335(6) Uani 1 1 d . . .
C30 C 0.1811(2) 0.62042(19) 0.12477(18) 0.0364(6) Uani 1 1 d . . .
H30 H 0.1869 0.6033 0.0584 0.044 Uiso 1 1 calc R . .
C31 C 0.09018(19) 0.68018(19) 0.15113(18) 0.0336(6) Uani 1 1 d . . .
C32 C 0.08281(19) 0.70429(19) 0.24840(18) 0.0341(6) Uani 1 1 d . A .
H32 H 0.0209 0.7449 0.2667 0.041 Uiso 1 1 calc R . .
C33 C 0.16242(19) 0.67127(18) 0.31997(18) 0.0322(6) Uani 1 1 d . . .
C37 C 0.3613(2) 0.5181(2) 0.16432(19) 0.0447(7) Uani 1 1 d . . .
H37 H 0.3979 0.484 0.2283 0.054 Uiso 1 1 calc R . .
C38 C 0.3331(3) 0.4316(2) 0.1069(2) 0.0569(8) Uani 1 1 d . . .
H38A H 0.2838 0.3894 0.1472 0.085 Uiso 1 1 calc R . .
H38B H 0.3981 0.3878 0.0943 0.085 Uiso 1 1 calc R . .
H38C H 0.2993 0.4625 0.0424 0.085 Uiso 1 1 calc R . .
C39 C 0.4389(2) 0.5835(3) 0.1047(2) 0.0612(9) Uani 1 1 d . . .
H39A H 0.5012 0.5387 0.0872 0.092 Uiso 1 1 calc R . .
H39B H 0.4616 0.6336 0.1454 0.092 Uiso 1 1 calc R . .
H39C H 0.4042 0.6208 0.0428 0.092 Uiso 1 1 calc R . .
C40 C 0.0014(2) 0.7188(2) 0.07475(19) 0.0379(6) Uani 1 1 d . . .
H40 H -0.0591 0.7525 0.111 0.045 Uiso 1 1 calc R . .
C41 C -0.0397(2) 0.6313(2) 0.0296(2) 0.0480(7) Uani 1 1 d . . .
H41A H -0.097 0.6594 -0.0186 0.072 Uiso 1 1 calc R . .
H41B H -0.0671 0.582 0.0835 0.072 Uiso 1 1 calc R . .
H41C H 0.0185 0.5957 -0.0052 0.072 Uiso 1 1 calc R . .
C42 C 0.0378(2) 0.8003(2) -0.0068(2) 0.0482(7) Uani 1 1 d . . .
H42A H -0.0205 0.8248 -0.055 0.072 Uiso 1 1 calc R . .
H42B H 0.099 0.7702 -0.0421 0.072 Uiso 1 1 calc R . .
H42C H 0.0586 0.8587 0.0238 0.072 Uiso 1 1 calc R . .
C43 C 0.2239(2) 0.3395(2) 0.6265(2) 0.0559(8) Uani 1 1 d . . .
H43A H 0.1846 0.2781 0.6259 0.067 Uiso 1 1 calc R . .
H43B H 0.2048 0.3896 0.565 0.067 Uiso 1 1 calc R . .
C44 C 0.1972(3) 0.3884(3) 0.7194(2) 0.0616(9) Uani 1 1 d . . .
H44A H 0.1248 0.3754 0.7436 0.074 Uiso 1 1 calc R . .
H44B H 0.2018 0.4641 0.7062 0.074 Uiso 1 1 calc R . .
C45 C 0.2812(3) 0.3351(3) 0.7952(3) 0.0718(10) Uani 1 1 d . . .
H45A H 0.3176 0.3868 0.825 0.086 Uiso 1 1 calc R . .
H45B H 0.2487 0.2895 0.8501 0.086 Uiso 1 1 calc R . .
C46 C 0.3585(3) 0.2723(3) 0.7357(2) 0.0589(8) Uani 1 1 d . . .
H46A H 0.4328 0.2815 0.7525 0.071 Uiso 1 1 calc R . .
H46B H 0.3485 0.1978 0.7514 0.071 Uiso 1 1 calc R . .
Mo1 Mo 0.453313(16) 0.441957(15) 0.533022(14) 0.02669(8) Uani 1 1 d . . .
N1 N 0.10382(17) 1.08514(16) 1.24878(16) 0.0410(5) Uani 1 1 d . . .
N2 N 0.2468(2) 0.6162(2) 0.8376(2) 0.0592(7) Uani 1 1 d . . .
O1 O 0.39121(12) 0.53573(12) 0.63924(11) 0.0293(4) Uani 1 1 d . . .
O2 O 0.32685(12) 0.49766(12) 0.43270(11) 0.0290(4) Uani 1 1 d . . .
O3 O 0.49224(13) 0.65775(12) 0.57050(11) 0.0301(4) Uani 1 1 d . . .
O4 O 0.57485(12) 0.38002(12) 0.63816(11) 0.0289(4) Uani 1 1 d . . .
O5 O 0.33650(15) 0.30977(15) 0.63059(14) 0.0491(5) Uani 1 1 d . . .
S1 S 0.33047(5) 0.82960(5) 0.89764(5) 0.03846(17) Uani 1 1 d . . .
C34A C 0.1524(2) 0.6956(2) 0.4277(2) 0.0445(7) Uani 0.358(6) 1 d PD A 1
H34A H 0.2255 0.6859 0.4578 0.053 Uiso 0.358(6) 1 calc PR A 1
C35A C 0.0876(8) 0.6124(8) 0.4864(6) 0.075(4) Uani 0.358(6) 1 d PD A 1
H35A H 0.1219 0.5433 0.4796 0.113 Uiso 0.358(6) 1 calc PR A 1
H35B H 0.0151 0.6205 0.4588 0.113 Uiso 0.358(6) 1 calc PR A 1
H35C H 0.0848 0.6208 0.5578 0.113 Uiso 0.358(6) 1 calc PR A 1
C36A C 0.1074(10) 0.7989(8) 0.4363(7) 0.082(4) Uani 0.358(6) 1 d PD A 1
H36A H 0.1044 0.8078 0.5076 0.123 Uiso 0.358(6) 1 calc PR A 1
H36B H 0.0352 0.8105 0.4077 0.123 Uiso 0.358(6) 1 calc PR A 1
H36C H 0.1518 0.8489 0.3996 0.123 Uiso 0.358(6) 1 calc PR A 1
C34B C 0.1524(2) 0.6956(2) 0.4277(2) 0.0445(7) Uani 0.642(6) 1 d PD A 2
H34B H 0.1832 0.6328 0.474 0.053 Uiso 0.642(6) 1 calc PR A 2
C35B C 0.0375(4) 0.7219(4) 0.4607(4) 0.0602(16) Uani 0.642(6) 1 d PD A 2
H35D H 0.0373 0.7363 0.5304 0.09 Uiso 0.642(6) 1 calc PR A 2
H35E H -0.0035 0.6632 0.4565 0.09 Uiso 0.642(6) 1 calc PR A 2
H35F H 0.0052 0.7832 0.4163 0.09 Uiso 0.642(6) 1 calc PR A 2
C36B C 0.2156(4) 0.7856(4) 0.4428(4) 0.0550(15) Uani 0.642(6) 1 d PD A 2
H36D H 0.2081 0.7988 0.5127 0.082 Uiso 0.642(6) 1 calc PR A 2
H36E H 0.1882 0.8479 0.397 0.082 Uiso 0.642(6) 1 calc PR A 2
H36F H 0.291 0.7677 0.4284 0.082 Uiso 0.642(6) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0301(13) 0.0327(14) 0.0271(13) -0.0077(10) -0.0016(11) -0.0014(11)
C2 0.0354(14) 0.0366(14) 0.0299(13) -0.0110(11) 0.0033(11) -0.0014(11)
C3 0.0482(17) 0.0392(15) 0.0384(15) -0.0188(12) 0.0063(14) -0.0048(13)
C4 0.0359(14) 0.0373(14) 0.0311(13) -0.0085(11) 0.0041(11) -0.0002(11)
C5 0.0357(14) 0.0399(15) 0.0354(14) -0.0123(11) 0.0029(11) -0.0013(12)
C6 0.0437(16) 0.0468(16) 0.0360(15) -0.0104(12) 0.0013(12) -0.0109(13)
C7 0.0410(15) 0.0424(15) 0.0419(15) -0.0143(12) 0.0021(13) -0.0074(12)
C8 0.0343(14) 0.0359(14) 0.0376(14) -0.0129(11) -0.0043(11) -0.0009(11)
C9 0.0338(14) 0.0386(15) 0.0363(14) -0.0129(11) -0.0021(11) -0.0020(11)
C10 0.0467(16) 0.0354(14) 0.0411(15) -0.0125(12) 0.0019(13) -0.0011(12)
C11 0.0513(17) 0.0375(15) 0.0376(15) -0.0074(12) 0.0057(13) -0.0069(13)
C12 0.0385(15) 0.0383(15) 0.0353(14) -0.0136(11) -0.0010(12) -0.0031(12)
C13 0.0420(15) 0.0367(14) 0.0405(15) -0.0141(12) -0.0013(12) -0.0044(12)
C14 0.0363(15) 0.0408(15) 0.0401(15) -0.0110(12) 0.0014(12) -0.0077(12)
C15 0.0404(15) 0.0345(14) 0.0432(15) -0.0124(12) 0.0036(12) -0.0050(12)
C16 0.0566(19) 0.0516(18) 0.0516(18) -0.0245(14) 0.0125(15) -0.0138(15)
C17 0.064(2) 0.057(2) 0.074(2) -0.0250(17) 0.0255(18) -0.0168(17)
C18 0.0442(18) 0.0499(19) 0.095(3) -0.0242(18) 0.0123(18) -0.0115(15)
C19 0.0439(17) 0.0495(18) 0.068(2) -0.0216(15) -0.0063(15) -0.0052(14)
C20 0.0478(17) 0.0393(15) 0.0479(16) -0.0108(13) -0.0055(13) -0.0049(13)
C21 0.0535(17) 0.0394(15) 0.0330(14) -0.0162(12) 0.0073(12) -0.0126(13)
C22 0.066(2) 0.0478(17) 0.0358(15) -0.0135(13) 0.0061(14) -0.0062(15)
C23 0.097(3) 0.0390(17) 0.056(2) -0.0077(15) 0.0274(19) -0.0019(17)
C24 0.089(3) 0.064(2) 0.071(2) -0.0370(19) 0.034(2) -0.047(2)
C25 0.072(2) 0.088(3) 0.068(2) -0.047(2) 0.0179(19) -0.040(2)
C26 0.0547(19) 0.064(2) 0.0541(18) -0.0250(15) 0.0022(15) -0.0152(15)
C27 0.0317(14) 0.0324(13) 0.0243(12) -0.0102(10) 0.0020(10) -0.0017(11)
C28 0.0328(13) 0.0299(13) 0.0279(12) -0.0059(10) -0.0007(10) -0.0066(11)
C29 0.0339(14) 0.0382(14) 0.0288(13) -0.0070(11) 0.0000(11) -0.0028(11)
C30 0.0404(15) 0.0449(15) 0.0249(13) -0.0088(11) -0.0014(11) -0.0031(12)
C31 0.0338(14) 0.0353(14) 0.0322(13) -0.0042(11) 0.0001(11) -0.0073(11)
C32 0.0313(14) 0.0343(14) 0.0375(14) -0.0098(11) 0.0027(11) -0.0013(11)
C33 0.0355(14) 0.0305(13) 0.0314(13) -0.0069(10) 0.0000(11) -0.0042(11)
C37 0.0439(16) 0.0612(18) 0.0277(14) -0.0129(12) -0.0028(12) 0.0103(14)
C38 0.064(2) 0.0562(19) 0.0510(18) -0.0202(15) 0.0109(15) 0.0086(16)
C39 0.0388(17) 0.088(2) 0.064(2) -0.0326(18) 0.0110(15) -0.0072(16)
C40 0.0340(14) 0.0432(15) 0.0357(14) -0.0059(12) -0.0051(11) -0.0005(12)
C41 0.0534(18) 0.0488(17) 0.0428(16) -0.0049(13) -0.0130(14) -0.0111(14)
C42 0.0474(17) 0.0508(17) 0.0454(16) -0.0013(13) -0.0135(13) -0.0082(14)
C43 0.0527(19) 0.062(2) 0.0534(19) 0.0002(15) 0.0002(15) -0.0228(16)
C44 0.0505(19) 0.073(2) 0.066(2) -0.0129(17) 0.0094(16) -0.0211(17)
C45 0.073(2) 0.093(3) 0.051(2) -0.0110(18) 0.0122(18) -0.017(2)
C46 0.062(2) 0.062(2) 0.0515(19) 0.0061(15) -0.0004(16) -0.0228(16)
Mo1 0.02879(13) 0.03009(13) 0.02277(12) -0.00649(8) 0.00079(8) -0.00682(9)
N1 0.0443(13) 0.0399(12) 0.0439(13) -0.0193(10) 0.0074(10) -0.0101(10)
N2 0.0682(18) 0.0596(16) 0.0579(16) -0.0276(13) 0.0259(15) -0.0204(14)
O1 0.0301(9) 0.0338(9) 0.0254(8) -0.0073(7) 0.0028(7) -0.0064(7)
O2 0.0290(9) 0.0321(9) 0.0271(8) -0.0050(7) 0.0001(7) -0.0076(7)
O3 0.0338(9) 0.0319(9) 0.0265(8) -0.0084(7) 0.0027(7) -0.0072(7)
O4 0.0302(9) 0.0314(9) 0.0257(8) -0.0040(7) 0.0011(7) -0.0061(7)
O5 0.0489(12) 0.0522(12) 0.0484(12) -0.0080(9) 0.0047(9) -0.0154(9)
S1 0.0420(4) 0.0380(4) 0.0390(4) -0.0164(3) 0.0068(3) -0.0064(3)
C34A 0.0489(17) 0.0522(17) 0.0331(14) -0.0155(12) 0.0004(12) 0.0041(14)
C35A 0.074(7) 0.110(9) 0.038(5) -0.012(5) 0.012(5) 0.008(6)
C36A 0.116(12) 0.082(8) 0.047(6) -0.033(5) -0.008(6) 0.030(7)
C34B 0.0489(17) 0.0522(17) 0.0331(14) -0.0155(12) 0.0004(12) 0.0041(14)
C35B 0.060(3) 0.080(4) 0.043(3) -0.022(3) 0.013(2) -0.003(3)
C36B 0.062(4) 0.061(3) 0.049(3) -0.032(2) -0.004(2) -0.002(3)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O3 1.270(3) . ?
C1 O1 1.276(3) . ?
C1 C2 1.473(3) . ?
C2 C4 1.352(3) . ?
C2 C3 1.434(4) . ?
C3 N2 1.154(4) . ?
C4 C5 1.428(3) . ?
C4 H4 0.95 . ?
C5 C6 1.373(4) . ?
C5 S1 1.734(3) . ?
C6 C7 1.389(4) . ?
C6 H6 0.95 . ?
C7 C8 1.368(4) . ?
C7 H7 0.95 . ?
C8 C9 1.462(4) . ?
C8 S1 1.729(3) . ?
C9 C10 1.393(4) . ?
C9 C14 1.395(4) . ?
C10 C11 1.379(4) . ?
C10 H10 0.95 . ?
C11 C12 1.395(4) . ?
C11 H11 0.95 . ?
C12 C13 1.397(4) . ?
C12 N1 1.404(3) . ?
C13 C14 1.382(4) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?
C15 C16 1.387(4) . ?
C15 C20 1.391(4) . ?
C15 N1 1.422(3) . ?
C16 C17 1.393(4) . ?
C16 H16 0.95 . ?
C17 C18 1.377(4) . ?
C17 H17 0.95 . ?
C18 C19 1.370(5) . ?
C18 H18 0.95 . ?
C19 C20 1.371(4) . ?
C19 H19 0.95 . ?
C20 H20 0.95 . ?
C21 C22 1.377(4) . ?
C21 C26 1.381(4) . ?
C21 N1 1.442(3) . ?
C22 C23 1.400(4) . ?
C22 H22 0.95 . ?
C23 C24 1.376(5) . ?
C23 H23 0.95 . ?
C24 C25 1.348(5) . ?
C24 H24 0.95 . ?
C25 C26 1.380(5) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C27 O4 1.267(3) 2_666 ?
C27 O2 1.277(3) . ?
C27 C28 1.495(3) . ?
C28 C33 1.402(3) . ?
C28 C29 1.403(3) . ?
C29 C30 1.389(3) . ?
C29 C37 1.523(4) . ?
C30 C31 1.394(3) . ?
C30 H30 0.95 . ?
C31 C32 1.387(3) . ?
C31 C40 1.521(3) . ?
C32 C33 1.387(3) . ?
C32 H32 0.95 . ?
C33 C34A 1.527(3) . ?
C37 C39 1.513(4) . ?
C37 C38 1.535(4) . ?
C37 H37 1 . ?
C38 H38A 0.98 . ?
C38 H38B 0.98 . ?
C38 H38C 0.98 . ?
C39 H39A 0.98 . ?
C39 H39B 0.98 . ?
C39 H39C 0.98 . ?
C40 C42 1.513(4) . ?
C40 C41 1.514(4) . ?
C40 H40 1 . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C41 H41C 0.98 . ?
C42 H42A 0.98 . ?
C42 H42B 0.98 . ?
C42 H42C 0.98 . ?
C43 O5 1.433(4) . ?
C43 C44 1.504(4) . ?
C43 H43A 0.99 . ?
C43 H43B 0.99 . ?
C44 C45 1.517(5) . ?
C44 H44A 0.99 . ?
C44 H44B 0.99 . ?
C45 C46 1.509(5) . ?
C45 H45A 0.99 . ?
C45 H45B 0.99 . ?
C46 O5 1.442(3) . ?
C46 H46A 0.99 . ?
C46 H46B 0.99 . ?
Mo1 O2 2.0977(15) . ?
Mo1 Mo1 2.1065(4) 2_666 ?
Mo1 O3 2.1082(16) 2_666 ?
Mo1 O4 2.1082(15) . ?
Mo1 O1 2.1107(16) . ?
O3 Mo1 2.1082(16) 2_666 ?
O4 C27 1.267(3) 2_666 ?
C34A C36A 1.434(9) . ?
C34A C35A 1.546(10) . ?
C34A H34A 1 . ?
C35A H35A 0.98 . ?
C35A H35B 0.98 . ?
C35A H35C 0.98 . ?
C36A H36A 0.98 . ?
C36A H36B 0.98 . ?
C36A H36C 0.98 . ?
C35B H35D 0.98 . ?
C35B H35E 0.98 . ?
C35B H35F 0.98 . ?
C36B H36D 0.98 . ?
C36B H36E 0.98 . ?
C36B H36F 0.98 . ?
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
O3 C1 O1 122.7(2) . . ?
O3 C1 C2 119.4(2) . . ?
O1 C1 C2 117.9(2) . . ?
C4 C2 C3 122.3(2) . . ?
C4 C2 C1 121.3(2) . . ?
C3 C2 C1 116.4(2) . . ?
N2 C3 C2 179.9(3) . . ?
C2 C4 C5 131.1(2) . . ?
C2 C4 H4 114.4 . . ?
C5 C4 H4 114.4 . . ?
C6 C5 C4 125.9(2) . . ?
C6 C5 S1 109.39(19) . . ?
C4 C5 S1 124.7(2) . . ?
C5 C6 C7 114.6(3) . . ?
C5 C6 H6 122.7 . . ?
C7 C6 H6 122.7 . . ?
C8 C7 C6 113.1(2) . . ?
C8 C7 H7 123.4 . . ?
C6 C7 H7 123.4 . . ?
C7 C8 C9 130.0(2) . . ?
C7 C8 S1 110.58(19) . . ?
C9 C8 S1 119.34(19) . . ?
C10 C9 C14 117.1(2) . . ?
C10 C9 C8 121.4(2) . . ?
C14 C9 C8 121.4(2) . . ?
C11 C10 C9 121.5(2) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 121.0(3) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 117.7(2) . . ?
C11 C12 N1 120.6(2) . . ?
C13 C12 N1 121.6(2) . . ?
C14 C13 C12 120.6(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C9 121.6(3) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
C16 C15 C20 118.3(3) . . ?
C16 C15 N1 118.9(2) . . ?
C20 C15 N1 122.7(2) . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 119.4(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C18 C19 C20 121.0(3) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C19 C20 C15 120.7(3) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
C22 C21 C26 120.4(3) . . ?
C22 C21 N1 120.3(2) . . ?
C26 C21 N1 119.3(3) . . ?
C21 C22 C23 119.0(3) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 121.3(3) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C25 C26 C21 119.9(3) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
O4 C27 O2 122.0(2) 2_666 . ?
O4 C27 C28 119.8(2) 2_666 . ?
O2 C27 C28 118.2(2) . . ?
C33 C28 C29 121.8(2) . . ?
C33 C28 C27 118.9(2) . . ?
C29 C28 C27 119.2(2) . . ?
C30 C29 C28 118.1(2) . . ?
C30 C29 C37 121.0(2) . . ?
C28 C29 C37 120.8(2) . . ?
C29 C30 C31 121.5(2) . . ?
C29 C30 H30 119.2 . . ?
C31 C30 H30 119.2 . . ?
C32 C31 C30 118.5(2) . . ?
C32 C31 C40 120.7(2) . . ?
C30 C31 C40 120.8(2) . . ?
C33 C32 C31 122.4(2) . . ?
C33 C32 H32 118.8 . . ?
C31 C32 H32 118.8 . . ?
C32 C33 C28 117.5(2) . . ?
C32 C33 C34A 122.1(2) . . ?
C28 C33 C34A 120.4(2) . . ?
C39 C37 C29 110.9(2) . . ?
C39 C37 C38 110.7(2) . . ?
C29 C37 C38 112.8(2) . . ?
C39 C37 H37 107.4 . . ?
C29 C37 H37 107.4 . . ?
C38 C37 H37 107.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C42 C40 C41 111.0(2) . . ?
C42 C40 C31 110.6(2) . . ?
C41 C40 C31 112.1(2) . . ?
C42 C40 H40 107.6 . . ?
C41 C40 H40 107.6 . . ?
C31 C40 H40 107.6 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C43 C44 106.2(2) . . ?
O5 C43 H43A 110.5 . . ?
C44 C43 H43A 110.5 . . ?
O5 C43 H43B 110.5 . . ?
C44 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
C43 C44 C45 103.5(3) . . ?
C43 C44 H44A 111.1 . . ?
C45 C44 H44A 111.1 . . ?
C43 C44 H44B 111.1 . . ?
C45 C44 H44B 111.1 . . ?
H44A C44 H44B 109 . . ?
C46 C45 C44 105.1(3) . . ?
C46 C45 H45A 110.7 . . ?
C44 C45 H45A 110.7 . . ?
C46 C45 H45B 110.7 . . ?
C44 C45 H45B 110.7 . . ?
H45A C45 H45B 108.8 . . ?
O5 C46 C45 106.7(2) . . ?
O5 C46 H46A 110.4 . . ?
C45 C46 H46A 110.4 . . ?
O5 C46 H46B 110.4 . . ?
C45 C46 H46B 110.4 . . ?
H46A C46 H46B 108.6 . . ?
O2 Mo1 Mo1 91.89(4) . 2_666 ?
O2 Mo1 O3 87.29(6) . 2_666 ?
Mo1 Mo1 O3 92.20(4) 2_666 2_666 ?
O2 Mo1 O4 176.78(6) . . ?
Mo1 Mo1 O4 91.32(4) 2_666 . ?
O3 Mo1 O4 92.92(6) 2_666 . ?
O2 Mo1 O1 91.74(6) . . ?
Mo1 Mo1 O1 91.27(4) 2_666 . ?
O3 Mo1 O1 176.42(6) 2_666 . ?
O4 Mo1 O1 87.86(6) . . ?
C12 N1 C15 121.7(2) . . ?
C12 N1 C21 118.9(2) . . ?
C15 N1 C21 117.7(2) . . ?
C1 O1 Mo1 117.12(15) . . ?
C27 O2 Mo1 117.25(14) . . ?
C1 O3 Mo1 116.55(15) . 2_666 ?
C27 O4 Mo1 117.51(14) 2_666 . ?
C43 O5 C46 104.4(2) . . ?
C8 S1 C5 92.33(13) . . ?
C36A C34A C33 115.0(4) . . ?
C36A C34A C35A 112.2(7) . . ?
C33 C34A C35A 106.4(4) . . ?
C36A C34A H34A 107.6 . . ?
C33 C34A H34A 107.6 . . ?
C35A C34A H34A 107.6 . . ?
C34A C35A H35A 109.5 . . ?
C34A C35A H35B 109.5 . . ?
H35A C35A H35B 109.5 . . ?
C34A C35A H35C 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C34A C36A H36A 109.5 . . ?
C34A C36A H36B 109.5 . . ?
H36A C36A H36B 109.5 . . ?
C34A C36A H36C 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
H35D C35B H35E 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
H36D C36B H36E 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
#----------------------------------------------------------------------------#
# PLATON/Squeeze #
#----------------------------------------------------------------------------#
loop_
_platon_squeeze_void_nr
1
_platon_squeeze_void_average_x   0.500
_platon_squeeze_void_average_y   1.000
_platon_squeeze_void_average_z   0.500
_platon_squeeze_void_volume      162
_platon_squeeze_void_count_electrons 33
_platon_squeeze_void_content     THF
_platon_squeeze_details          
;
Several residual "Q" peaks remained in the difference map after final
refinement that could not be modeled as solvent. The PLATON squeeze
program was utilized to remove the residual electron density. The program
removed 33 electrons from the solvent accessible void which correlates to
one disordered THF molecule.
;


data_sharlene2
_database_code_depnum_ccdc_archive 'CCDC 919556'
#TrackingRef 'Master_archive.cif'
_audit_creation_date             2013-01-04T12:38:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Chisholm 1892'
_chemical_formula_moiety         
'C84 H92 Mo2 N4 O10, C76 H76 Mo2 N4 O8, 4(C4 H8 O)'
_chemical_formula_sum            'C176 H200 Mo4 N8 O22'
_chemical_formula_weight         3163.2
_chemical_compound_source        'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   12.843(3)
_cell_length_b                   16.816(3)
_cell_length_c                   21.696(4)
_cell_angle_alpha                74.31(3)
_cell_angle_beta                 76.48(3)
_cell_angle_gamma                72.72(3)
_cell_volume                     4247.0(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    14939
_cell_measurement_theta_min      1.018
_cell_measurement_theta_max      25.028
_cell_measurement_wavelength     0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_special_details           
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.581724E-1
_diffrn_orient_matrix_ub_12      -0.397376E-1
_diffrn_orient_matrix_ub_13      -0.246276E-1
_diffrn_orient_matrix_ub_21      0.474633E-1
_diffrn_orient_matrix_ub_22      0.413492E-1
_diffrn_orient_matrix_ub_23      -0.130064E-1
_diffrn_orient_matrix_ub_31      0.346885E-1
_diffrn_orient_matrix_ub_32      -0.279388E-1
_diffrn_orient_matrix_ub_33      0.397742E-1
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_number            14467
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             14467
_reflns_number_gt                9794
_reflns_threshold_expression     >2\s(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+1.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         14467
_refine_ls_number_parameters     946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.059
_refine_ls_wR_factor_ref         0.1682
_refine_ls_wR_factor_gt          0.1544
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_restrained_S_all      1.08
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.085
#----------------------------------------------------------------------------#
# SQEEZE RESULTS #
#----------------------------------------------------------------------------#
_platon_squeeze_void_nr          1
_platon_squeeze_void_average_x   0.500
_platon_squeeze_void_average_y   0.500
_platon_squeeze_void_average_z   0.000
_platon_squeeze_void_volume      290
_platon_squeeze_void_count_electrons 43
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.94397(3) 0.55468(2) 0.478688(19) 0.03421(13) Uani 1 1 d . . .
Mo2 Mo 0.44771(3) 0.95839(2) 0.011163(19) 0.03856(14) Uani 1 1 d . . .
N1 N 1.0017(3) 0.9938(2) 0.71928(18) 0.0407(9) Uani 1 1 d . . .
N2 N 1.2423(5) 0.5716(3) 0.6655(3) 0.0916(19) Uani 1 1 d . . .
N3 N 0.3106(3) 1.0222(2) -0.45868(18) 0.0409(9) Uani 1 1 d . . .
N4 N 0.5427(5) 1.1851(3) -0.2690(2) 0.0738(15) Uani 1 1 d . . .
O1 O 0.9873(2) 0.63298(17) 0.52413(14) 0.0362(7) Uani 1 1 d . . .
O2 O 1.1080(2) 0.51712(17) 0.56936(15) 0.0387(7) Uani 1 1 d . . .
O3 O 0.9348(2) 0.42366(17) 0.60324(14) 0.0374(7) Uani 1 1 d . . .
O4 O 0.8173(2) 0.53924(17) 0.55912(15) 0.0376(7) Uani 1 1 d . . .
O5 O 0.4188(2) 0.99154(19) -0.08567(14) 0.0402(7) Uani 1 1 d . . .
O6 O 0.5286(3) 1.08042(18) -0.10887(14) 0.0414(7) Uani 1 1 d . . .
O7 O 0.5789(3) 0.85611(19) -0.01266(15) 0.0442(8) Uani 1 1 d . . .
O8 O 0.6903(2) 0.94414(19) -0.03647(15) 0.0434(8) Uani 1 1 d . . .
O100 O 0.2991(4) 0.8772(3) 0.0369(2) 0.0857(14) Uani 1 1 d . . .
O200 O 0.8155(3) 0.68038(19) 0.40545(16) 0.0481(8) Uani 1 1 d . . .
C1 C 1.0585(4) 0.5966(3) 0.5620(2) 0.0359(10) Uani 1 1 d . . .
C2 C 1.0822(4) 0.6474(3) 0.6008(2) 0.0401(11) Uani 1 1 d . . .
C3 C 1.0183(4) 0.7276(3) 0.6015(2) 0.0385(11) Uani 1 1 d . . .
H3A H 0.9624 0.745 0.5752 0.046 Uiso 1 1 calc R . .
C4 C 1.0186(4) 0.7918(3) 0.6342(2) 0.0370(11) Uani 1 1 d . . .
C5 C 0.9427(4) 0.8707(3) 0.6209(2) 0.0409(11) Uani 1 1 d . . .
H5A H 0.893 0.8788 0.5922 0.049 Uiso 1 1 calc R . .
C6 C 0.9376(4) 0.9363(3) 0.6478(2) 0.0420(11) Uani 1 1 d . . .
H6A H 0.8857 0.9894 0.6369 0.05 Uiso 1 1 calc R . .
C7 C 1.0084(4) 0.9264(3) 0.6914(2) 0.0391(11) Uani 1 1 d . . .
C8 C 1.0857(4) 0.8474(3) 0.7051(2) 0.0420(11) Uani 1 1 d . . .
H8A H 1.1351 0.8395 0.734 0.05 Uiso 1 1 calc R . .
C9 C 1.0908(4) 0.7817(3) 0.6776(2) 0.0416(11) Uani 1 1 d . . .
H9A H 1.1434 0.7288 0.6877 0.05 Uiso 1 1 calc R . .
C10 C 0.9576(4) 1.0795(3) 0.6853(2) 0.0416(12) Uani 1 1 d . . .
C11 C 0.8601(4) 1.1300(3) 0.7118(3) 0.0553(14) Uani 1 1 d . . .
H11A H 0.8213 1.1084 0.753 0.066 Uiso 1 1 calc R . .
C12 C 0.8194(5) 1.2113(3) 0.6785(3) 0.0597(15) Uani 1 1 d . . .
H12A H 0.7528 1.246 0.697 0.072 Uiso 1 1 calc R . .
C13 C 0.8743(4) 1.2424(3) 0.6191(3) 0.0505(13) Uani 1 1 d . . .
H13A H 0.8453 1.2985 0.596 0.061 Uiso 1 1 calc R . .
C14 C 0.9717(4) 1.1927(3) 0.5927(3) 0.0476(13) Uani 1 1 d . . .
H14A H 1.0098 1.2148 0.5514 0.057 Uiso 1 1 calc R . .
C15 C 1.0140(4) 1.1116(3) 0.6255(2) 0.0418(11) Uani 1 1 d . . .
H15A H 1.0816 1.0777 0.6073 0.05 Uiso 1 1 calc R . .
C16 C 1.0347(4) 0.9820(3) 0.7804(2) 0.0446(12) Uani 1 1 d . . .
C17 C 1.0817(4) 1.0424(3) 0.7898(3) 0.0527(13) Uani 1 1 d . . .
H17A H 1.0918 1.09 0.7556 0.063 Uiso 1 1 calc R . .
C18 C 1.1130(5) 1.0333(4) 0.8478(3) 0.0688(17) Uani 1 1 d . . .
H18A H 1.1452 1.0743 0.8534 0.083 Uiso 1 1 calc R . .
C19 C 1.0983(5) 0.9652(5) 0.8983(3) 0.0800(19) Uani 1 1 d . . .
H19A H 1.1211 0.9584 0.9385 0.096 Uiso 1 1 calc R . .
C20 C 1.0494(6) 0.9067(4) 0.8890(3) 0.0760(18) Uani 1 1 d . . .
H20A H 1.0375 0.8599 0.9236 0.091 Uiso 1 1 calc R . .
C21 C 1.0185(4) 0.9152(3) 0.8317(2) 0.0532(13) Uani 1 1 d . . .
H21A H 0.985 0.8745 0.8266 0.064 Uiso 1 1 calc R . .
C22 C 1.1712(5) 0.6048(3) 0.6370(3) 0.0567(15) Uani 1 1 d . . .
C23 C 0.8407(4) 0.4750(3) 0.6059(2) 0.0372(11) Uani 1 1 d . . .
C24 C 0.7542(4) 0.4597(3) 0.6641(2) 0.0433(12) Uani 1 1 d . . .
C25 C 0.7718(4) 0.4571(3) 0.7255(2) 0.0503(13) Uani 1 1 d . . .
C26 C 0.6916(5) 0.4391(4) 0.7787(3) 0.0642(15) Uani 1 1 d . . .
H26A H 0.7023 0.4391 0.8205 0.077 Uiso 1 1 calc R . .
C27 C 0.5955(5) 0.4209(4) 0.7726(3) 0.0634(15) Uani 1 1 d . . .
C28 C 0.5802(4) 0.4245(3) 0.7109(3) 0.0613(15) Uani 1 1 d . . .
H28A H 0.5152 0.4125 0.7059 0.074 Uiso 1 1 calc R . .
C29 C 0.6563(4) 0.4449(3) 0.6560(3) 0.0483(12) Uani 1 1 d . . .
C30 C 0.4680(4) 1.0447(3) -0.1253(2) 0.0400(11) Uani 1 1 d . . .
C31 C 0.4554(4) 1.0652(3) -0.1946(2) 0.0399(11) Uani 1 1 d . . .
C32 C 0.4056(4) 1.0201(3) -0.2163(2) 0.0394(11) Uani 1 1 d . . .
H32A H 0.3779 0.9778 -0.1831 0.047 Uiso 1 1 calc R . .
C33 C 0.3861(4) 1.0235(3) -0.2800(2) 0.0383(11) Uani 1 1 d . . .
C34 C 0.3305(4) 0.9664(3) -0.2853(2) 0.0425(11) Uani 1 1 d . . .
H34A H 0.3093 0.9265 -0.2475 0.051 Uiso 1 1 calc R . .
C35 C 0.3055(4) 0.9659(3) -0.3435(2) 0.0397(11) Uani 1 1 d . . .
H35A H 0.2672 0.9263 -0.3453 0.048 Uiso 1 1 calc R . .
C36 C 0.3363(4) 1.0236(3) -0.4001(2) 0.0363(11) Uani 1 1 d . . .
C37 C 0.3933(4) 1.0799(3) -0.3951(2) 0.0378(11) Uani 1 1 d . . .
H37A H 0.4157 1.1191 -0.4331 0.045 Uiso 1 1 calc R . .
C38 C 0.4179(3) 1.0804(3) -0.3371(2) 0.0359(10) Uani 1 1 d . . .
H38A H 0.4569 1.1196 -0.3355 0.043 Uiso 1 1 calc R . .
C39 C 0.2994(4) 0.9439(3) -0.4686(2) 0.0398(11) Uani 1 1 d . . .
C40 C 0.3814(4) 0.8701(3) -0.4597(2) 0.0483(12) Uani 1 1 d . . .
H40A H 0.4461 0.8691 -0.4451 0.058 Uiso 1 1 calc R . .
C41 C 0.3696(5) 0.7974(3) -0.4719(3) 0.0631(15) Uani 1 1 d . . .
H41A H 0.4262 0.7461 -0.4652 0.076 Uiso 1 1 calc R . .
C42 C 0.2771(6) 0.7981(4) -0.4935(3) 0.0686(17) Uani 1 1 d . . .
H42A H 0.2702 0.7475 -0.502 0.082 Uiso 1 1 calc R . .
C43 C 0.1949(5) 0.8714(4) -0.5029(3) 0.0643(16) Uani 1 1 d . . .
H43A H 0.131 0.872 -0.5181 0.077 Uiso 1 1 calc R . .
C44 C 0.2051(4) 0.9450(3) -0.4901(2) 0.0523(13) Uani 1 1 d . . .
H44A H 0.1478 0.9959 -0.4961 0.063 Uiso 1 1 calc R . .
C45 C 0.3125(4) 1.0916(3) -0.5145(2) 0.0373(11) Uani 1 1 d . . .
C46 C 0.3599(4) 1.0745(3) -0.5754(2) 0.0437(12) Uani 1 1 d . . .
H46A H 0.3906 1.0172 -0.58 0.052 Uiso 1 1 calc R . .
C47 C 0.3627(4) 1.1399(4) -0.6287(2) 0.0584(15) Uani 1 1 d . . .
H47A H 0.3941 1.1278 -0.6704 0.07 Uiso 1 1 calc R . .
C48 C 0.3196(5) 1.2245(3) -0.6223(3) 0.0593(15) Uani 1 1 d . . .
H48A H 0.3237 1.2699 -0.6592 0.071 Uiso 1 1 calc R . .
C49 C 0.2710(4) 1.2413(3) -0.5618(3) 0.0525(13) Uani 1 1 d . . .
H49A H 0.2402 1.2988 -0.5575 0.063 Uiso 1 1 calc R . .
C50 C 0.2665(4) 1.1762(3) -0.5080(2) 0.0434(12) Uani 1 1 d . . .
H50A H 0.2324 1.1884 -0.4666 0.052 Uiso 1 1 calc R . .
C51 C 0.5050(4) 1.1321(3) -0.2363(2) 0.0495(13) Uani 1 1 d . . .
C52 C 0.6733(4) 0.8713(3) -0.0328(2) 0.0426(12) Uani 1 1 d . . .
C53 C 0.7695(4) 0.8042(3) -0.0565(3) 0.0515(13) Uani 1 1 d . . .
C54 C 0.7814(5) 0.7962(4) -0.1203(3) 0.0593(15) Uani 1 1 d . . .
C55 C 0.8731(6) 0.7356(5) -0.1424(4) 0.088(2) Uani 1 1 d . . .
H55A H 0.8826 0.7284 -0.1855 0.106 Uiso 1 1 calc R . .
C56 C 0.9507(6) 0.6858(5) -0.1041(5) 0.102(3) Uani 1 1 d . . .
C57 C 0.9348(5) 0.6953(4) -0.0409(4) 0.091(2) Uani 1 1 d . . .
H57A H 0.9868 0.6601 -0.0138 0.109 Uiso 1 1 calc R . .
C58 C 0.8448(5) 0.7550(4) -0.0157(3) 0.0708(17) Uani 1 1 d . . .
C101 C 0.3110(7) 0.8060(5) 0.0137(4) 0.109(3) Uani 1 1 d . . .
H10A H 0.3851 0.767 0.0176 0.13 Uiso 1 1 calc R . .
H10B H 0.3028 0.8225 -0.0327 0.13 Uiso 1 1 calc R . .
C102 C 0.2217(8) 0.7622(6) 0.0539(6) 0.148(4) Uani 1 1 d . . .
H10C H 0.2535 0.7005 0.0691 0.178 Uiso 1 1 calc R . .
H10D H 0.1638 0.7697 0.0282 0.178 Uiso 1 1 calc R . .
C103 C 0.1740(9) 0.8059(6) 0.1113(6) 0.168(5) Uani 1 1 d . . .
H10E H 0.0921 0.8208 0.1189 0.201 Uiso 1 1 calc R . .
H10F H 0.2005 0.769 0.1515 0.201 Uiso 1 1 calc R . .
C104 C 0.2153(6) 0.8809(4) 0.0909(4) 0.099(2) Uani 1 1 d . . .
H10G H 0.1538 0.9314 0.0803 0.119 Uiso 1 1 calc R . .
H10H H 0.2441 0.8878 0.1272 0.119 Uiso 1 1 calc R . .
C201 C 0.7134(4) 0.6665(3) 0.3998(3) 0.0720(19) Uani 1 1 d . . .
H20B H 0.6503 0.714 0.4107 0.086 Uiso 1 1 calc R . .
H20C H 0.7012 0.6126 0.4293 0.086 Uiso 1 1 calc R . .
C202 C 0.7250(7) 0.6618(4) 0.3307(4) 0.097(3) Uani 1 1 d . . .
H20D H 0.7584 0.6026 0.3249 0.116 Uiso 1 1 calc R . .
H20E H 0.6523 0.6826 0.3161 0.116 Uiso 1 1 calc R . .
C203 C 0.7993(6) 0.7186(5) 0.2945(3) 0.093(2) Uani 1 1 d . . .
H20F H 0.8544 0.6924 0.2607 0.112 Uiso 1 1 calc R . .
H20G H 0.756 0.7745 0.2734 0.112 Uiso 1 1 calc R . .
C204 C 0.8547(4) 0.7288(3) 0.3434(2) 0.0548(14) Uani 1 1 d . . .
H20H H 0.9358 0.7078 0.3319 0.066 Uiso 1 1 calc R . .
H20I H 0.8374 0.7897 0.3448 0.066 Uiso 1 1 calc R . .
C250 C 0.8744(4) 0.4771(4) 0.7358(3) 0.0587(14) Uani 1 1 d . . .
H25A H 0.9311 0.4701 0.696 0.07 Uiso 1 1 calc R . .
C251 C 0.8512(6) 0.5682(4) 0.7408(4) 0.113(3) Uani 1 1 d . . .
H25B H 0.9186 0.5792 0.7468 0.169 Uiso 1 1 calc R . .
H25C H 0.7928 0.5788 0.7779 0.169 Uiso 1 1 calc R . .
H25D H 0.8273 0.6061 0.7009 0.169 Uiso 1 1 calc R . .
C252 C 0.9244(5) 0.4172(4) 0.7919(3) 0.0803(19) Uani 1 1 d . . .
H25E H 0.9388 0.3584 0.7873 0.12 Uiso 1 1 calc R . .
H25F H 0.8733 0.4248 0.8324 0.12 Uiso 1 1 calc R . .
H25G H 0.9941 0.4292 0.7929 0.12 Uiso 1 1 calc R . .
C270 C 0.5104(6) 0.3982(4) 0.8331(4) 0.086(2) Uani 1 1 d . . .
H27A H 0.5317 0.41 0.8706 0.104 Uiso 1 1 calc R . .
C271 C 0.5117(7) 0.3048(5) 0.8490(4) 0.133(4) Uani 1 1 d . . .
H27B H 0.4578 0.2927 0.8883 0.199 Uiso 1 1 calc R . .
H27C H 0.5857 0.2702 0.8565 0.199 Uiso 1 1 calc R . .
H27D H 0.4924 0.291 0.8128 0.199 Uiso 1 1 calc R . .
C272 C 0.3970(6) 0.4512(6) 0.8268(5) 0.184(6) Uani 1 1 d . . .
H27E H 0.3461 0.4354 0.8666 0.276 Uiso 1 1 calc R . .
H27F H 0.3741 0.4419 0.7898 0.276 Uiso 1 1 calc R . .
H27G H 0.3958 0.5116 0.8197 0.276 Uiso 1 1 calc R . .
C290 C 0.6339(4) 0.4489(3) 0.5893(3) 0.0532(13) Uani 1 1 d . . .
H29A H 0.7065 0.4403 0.5593 0.064 Uiso 1 1 calc R . .
C291 C 0.5788(5) 0.3797(4) 0.5892(3) 0.0713(17) Uani 1 1 d . . .
H29B H 0.567 0.3849 0.5451 0.107 Uiso 1 1 calc R . .
H29C H 0.5074 0.3866 0.6184 0.107 Uiso 1 1 calc R . .
H29D H 0.6266 0.3233 0.604 0.107 Uiso 1 1 calc R . .
C292 C 0.5624(5) 0.5364(3) 0.5627(3) 0.0690(16) Uani 1 1 d . . .
H29E H 0.5495 0.5379 0.5196 0.104 Uiso 1 1 calc R . .
H29F H 0.6003 0.5804 0.5595 0.104 Uiso 1 1 calc R . .
H29G H 0.4914 0.547 0.5919 0.104 Uiso 1 1 calc R . .
C540 C 0.6974(5) 0.8490(4) -0.1620(3) 0.0752(18) Uani 1 1 d . . .
H54A H 0.6362 0.8793 -0.1321 0.09 Uiso 1 1 calc R . .
C541 C 0.7366(6) 0.9182(6) -0.2123(5) 0.151(4) Uani 1 1 d . . .
H54B H 0.678 0.9515 -0.2376 0.226 Uiso 1 1 calc R . .
H54C H 0.8021 0.8932 -0.2411 0.226 Uiso 1 1 calc R . .
H54D H 0.7557 0.9555 -0.1912 0.226 Uiso 1 1 calc R . .
C542 C 0.6449(13) 0.7989(7) -0.1861(6) 0.221(7) Uani 1 1 d . . .
H54E H 0.5898 0.8376 -0.2122 0.332 Uiso 1 1 calc R . .
H54F H 0.6087 0.7626 -0.1492 0.332 Uiso 1 1 calc R . .
H54G H 0.7015 0.7631 -0.2129 0.332 Uiso 1 1 calc R . .
C560 C 1.0516(7) 0.6212(6) -0.1312(7) 0.192(7) Uani 1 1 d . . .
H56A H 1.0386 0.6384 -0.1772 0.23 Uiso 1 1 calc R . .
C561 C 1.0442(9) 0.5431(8) -0.1201(8) 0.239(9) Uani 1 1 d . . .
H56B H 1.1105 0.5095 -0.143 0.359 Uiso 1 1 calc R . .
H56C H 0.9787 0.5423 -0.1356 0.359 Uiso 1 1 calc R . .
H56D H 1.0377 0.5185 -0.0734 0.359 Uiso 1 1 calc R . .
C562 C 1.1492(8) 0.6477(6) -0.1425(7) 0.217(7) Uani 1 1 d . . .
H56E H 1.2106 0.6067 -0.1624 0.326 Uiso 1 1 calc R . .
H56F H 1.1649 0.6508 -0.1012 0.326 Uiso 1 1 calc R . .
H56G H 1.1405 0.7041 -0.1718 0.326 Uiso 1 1 calc R . .
C580 C 0.8270(8) 0.7646(6) 0.0536(4) 0.121(3) Uani 1 1 d . . .
H58A H 0.7631 0.8157 0.0559 0.145 Uiso 1 1 calc R . .
C581 C 0.9092(14) 0.7862(10) 0.0699(5) 0.241(8) Uani 1 1 d . . .
H58B H 0.8901 0.7907 0.1155 0.362 Uiso 1 1 calc R . .
H58C H 0.9183 0.8413 0.0423 0.362 Uiso 1 1 calc R . .
H58D H 0.9784 0.7424 0.0637 0.362 Uiso 1 1 calc R . .
C582 C 0.7925(14) 0.7027(12) 0.0998(6) 0.289(11) Uani 1 1 d . . .
H58E H 0.7811 0.7164 0.1424 0.433 Uiso 1 1 calc R . .
H58F H 0.8484 0.6485 0.0988 0.433 Uiso 1 1 calc R . .
H58G H 0.7228 0.6977 0.092 0.433 Uiso 1 1 calc R . .
O300 O 0.3287(5) 0.7604(4) 0.7589(4) 0.135(2) Uani 1 1 d . . .
C303 C 0.4997(9) 0.6602(6) 0.7790(6) 0.154(4) Uani 1 1 d . . .
H30A H 0.5675 0.6808 0.7704 0.185 Uiso 1 1 calc R . .
H30B H 0.5106 0.6043 0.81 0.185 Uiso 1 1 calc R . .
C302 C 0.4734(10) 0.6532(6) 0.7170(7) 0.170(5) Uani 1 1 d . . .
H30C H 0.538 0.6542 0.6817 0.204 Uiso 1 1 calc R . .
H30D H 0.4503 0.6 0.723 0.204 Uiso 1 1 calc R . .
C304 C 0.4002(10) 0.7239(8) 0.8055(7) 0.180(5) Uani 1 1 d . . .
H30E H 0.3607 0.695 0.8462 0.216 Uiso 1 1 calc R . .
H30F H 0.4244 0.7692 0.8152 0.216 Uiso 1 1 calc R . .
C301 C 0.3837(11) 0.7273(10) 0.7030(7) 0.252(9) Uani 1 1 d . . .
H30G H 0.413 0.772 0.6695 0.303 Uiso 1 1 calc R . .
H30H H 0.3299 0.7119 0.6852 0.303 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0371(2) 0.0234(2) 0.0440(3) -0.00777(17) -0.01412(18) -0.00411(16)
Mo2 0.0450(3) 0.0398(2) 0.0325(2) -0.00886(18) -0.00965(19) -0.00968(19)
N1 0.051(2) 0.032(2) 0.041(2) -0.0125(17) -0.0122(19) -0.0066(18)
N2 0.099(4) 0.050(3) 0.146(5) -0.039(3) -0.083(4) 0.016(3)
N3 0.050(2) 0.039(2) 0.037(2) -0.0109(18) -0.0142(18) -0.0089(18)
N4 0.107(4) 0.082(4) 0.050(3) 0.002(3) -0.028(3) -0.054(3)
O1 0.0409(18) 0.0270(15) 0.0445(19) -0.0092(13) -0.0162(15) -0.0059(13)
O2 0.0374(18) 0.0278(16) 0.054(2) -0.0111(14) -0.0165(15) -0.0042(14)
O3 0.0368(18) 0.0267(15) 0.0479(19) -0.0058(13) -0.0147(15) -0.0028(14)
O4 0.0339(17) 0.0303(16) 0.050(2) -0.0120(15) -0.0131(15) -0.0021(13)
O5 0.0458(19) 0.0430(18) 0.0347(18) -0.0091(15) -0.0095(15) -0.0126(15)
O6 0.050(2) 0.0415(18) 0.0357(18) -0.0066(14) -0.0129(15) -0.0133(15)
O7 0.049(2) 0.0420(18) 0.0419(19) -0.0097(15) -0.0104(16) -0.0096(16)
O8 0.0450(19) 0.0447(19) 0.0411(19) -0.0126(15) -0.0093(15) -0.0075(15)
O100 0.090(3) 0.081(3) 0.100(3) -0.048(3) 0.022(3) -0.045(3)
O200 0.049(2) 0.0396(18) 0.056(2) -0.0076(16) -0.0178(17) -0.0064(15)
C1 0.036(3) 0.032(3) 0.045(3) -0.013(2) -0.007(2) -0.012(2)
C2 0.043(3) 0.029(2) 0.051(3) -0.008(2) -0.017(2) -0.007(2)
C3 0.044(3) 0.032(2) 0.041(3) -0.001(2) -0.015(2) -0.011(2)
C4 0.042(3) 0.030(2) 0.041(3) -0.008(2) -0.013(2) -0.007(2)
C5 0.043(3) 0.037(3) 0.042(3) -0.008(2) -0.015(2) -0.003(2)
C6 0.043(3) 0.035(3) 0.048(3) -0.013(2) -0.011(2) -0.002(2)
C7 0.043(3) 0.035(2) 0.042(3) -0.010(2) -0.006(2) -0.012(2)
C8 0.043(3) 0.037(3) 0.048(3) -0.012(2) -0.015(2) -0.006(2)
C9 0.045(3) 0.028(2) 0.050(3) -0.008(2) -0.015(2) -0.002(2)
C10 0.050(3) 0.029(2) 0.051(3) -0.015(2) -0.016(2) -0.007(2)
C11 0.060(3) 0.048(3) 0.056(3) -0.018(3) -0.001(3) -0.010(3)
C12 0.056(3) 0.035(3) 0.087(4) -0.023(3) -0.011(3) -0.001(3)
C13 0.052(3) 0.030(3) 0.076(4) -0.012(3) -0.025(3) -0.009(2)
C14 0.052(3) 0.044(3) 0.055(3) -0.005(2) -0.018(3) -0.023(3)
C15 0.048(3) 0.036(3) 0.047(3) -0.012(2) -0.014(2) -0.012(2)
C16 0.044(3) 0.043(3) 0.048(3) -0.018(2) -0.008(2) -0.004(2)
C17 0.061(3) 0.048(3) 0.053(3) -0.021(3) -0.011(3) -0.011(3)
C18 0.068(4) 0.080(4) 0.073(4) -0.040(4) -0.022(3) -0.012(3)
C19 0.090(5) 0.100(5) 0.056(4) -0.025(4) -0.029(4) -0.013(4)
C20 0.104(5) 0.069(4) 0.054(4) -0.003(3) -0.022(4) -0.023(4)
C21 0.066(4) 0.049(3) 0.046(3) -0.014(3) -0.016(3) -0.010(3)
C22 0.063(4) 0.032(3) 0.085(4) -0.026(3) -0.035(3) 0.003(3)
C23 0.042(3) 0.029(2) 0.046(3) -0.011(2) -0.014(2) -0.008(2)
C24 0.040(3) 0.039(3) 0.049(3) -0.006(2) -0.014(2) -0.006(2)
C25 0.049(3) 0.054(3) 0.047(3) -0.013(2) -0.012(3) -0.009(2)
C26 0.063(4) 0.078(4) 0.052(4) -0.021(3) -0.009(3) -0.012(3)
C27 0.047(3) 0.064(4) 0.076(4) -0.025(3) 0.006(3) -0.013(3)
C28 0.046(3) 0.068(4) 0.076(4) -0.028(3) -0.009(3) -0.012(3)
C29 0.035(3) 0.050(3) 0.060(3) -0.015(2) -0.008(3) -0.009(2)
C30 0.043(3) 0.042(3) 0.034(3) -0.010(2) -0.006(2) -0.007(2)
C31 0.043(3) 0.042(3) 0.033(3) -0.008(2) -0.010(2) -0.004(2)
C32 0.041(3) 0.040(3) 0.038(3) -0.007(2) -0.010(2) -0.009(2)
C33 0.041(3) 0.042(3) 0.033(3) -0.010(2) -0.011(2) -0.004(2)
C34 0.047(3) 0.040(3) 0.041(3) -0.008(2) -0.009(2) -0.010(2)
C35 0.046(3) 0.037(3) 0.040(3) -0.007(2) -0.013(2) -0.012(2)
C36 0.035(3) 0.038(2) 0.036(3) -0.014(2) -0.008(2) -0.003(2)
C37 0.040(3) 0.035(2) 0.034(3) -0.008(2) -0.005(2) -0.005(2)
C38 0.037(3) 0.037(2) 0.038(3) -0.014(2) -0.009(2) -0.007(2)
C39 0.051(3) 0.045(3) 0.032(3) -0.013(2) -0.008(2) -0.019(2)
C40 0.050(3) 0.050(3) 0.046(3) -0.020(2) -0.008(2) -0.007(3)
C41 0.071(4) 0.049(3) 0.069(4) -0.022(3) -0.007(3) -0.010(3)
C42 0.094(5) 0.061(4) 0.067(4) -0.032(3) 0.003(4) -0.038(4)
C43 0.077(4) 0.080(4) 0.051(3) -0.020(3) -0.007(3) -0.039(4)
C44 0.061(3) 0.060(3) 0.044(3) -0.016(3) -0.015(3) -0.017(3)
C45 0.038(3) 0.039(3) 0.032(3) -0.006(2) -0.009(2) -0.006(2)
C46 0.036(3) 0.048(3) 0.043(3) -0.014(2) -0.010(2) 0.001(2)
C47 0.058(3) 0.076(4) 0.033(3) -0.008(3) -0.005(2) -0.010(3)
C48 0.068(4) 0.052(3) 0.046(3) 0.003(3) -0.013(3) -0.006(3)
C49 0.054(3) 0.038(3) 0.060(4) -0.005(3) -0.017(3) -0.003(2)
C50 0.038(3) 0.049(3) 0.041(3) -0.014(2) -0.011(2) -0.001(2)
C51 0.068(4) 0.055(3) 0.036(3) -0.010(3) -0.019(3) -0.023(3)
C52 0.054(3) 0.044(3) 0.030(3) -0.009(2) -0.012(2) -0.008(2)
C53 0.054(3) 0.039(3) 0.061(4) -0.013(2) -0.009(3) -0.008(2)
C54 0.064(4) 0.066(4) 0.055(4) -0.027(3) 0.009(3) -0.029(3)
C55 0.081(5) 0.082(5) 0.105(6) -0.058(4) 0.034(5) -0.032(4)
C56 0.068(5) 0.061(4) 0.171(9) -0.056(5) 0.043(6) -0.026(4)
C57 0.061(4) 0.054(4) 0.135(7) -0.010(4) -0.015(4) 0.007(3)
C58 0.065(4) 0.055(4) 0.085(5) -0.013(3) -0.018(3) -0.002(3)
C101 0.102(6) 0.101(6) 0.133(7) -0.054(5) -0.004(5) -0.026(5)
C102 0.135(8) 0.132(8) 0.203(11) -0.054(8) 0.007(8) -0.083(7)
C103 0.152(9) 0.122(8) 0.236(13) -0.092(8) 0.072(9) -0.077(7)
C104 0.089(5) 0.088(5) 0.111(6) -0.036(4) 0.031(5) -0.032(4)
C201 0.045(3) 0.046(3) 0.111(6) 0.011(3) -0.025(3) -0.007(3)
C202 0.133(7) 0.060(4) 0.125(6) -0.007(4) -0.091(5) -0.024(4)
C203 0.071(5) 0.147(7) 0.072(5) -0.043(5) -0.016(4) -0.021(5)
C204 0.056(3) 0.052(3) 0.055(3) 0.000(3) -0.022(3) -0.012(3)
C250 0.056(3) 0.077(4) 0.048(3) -0.015(3) -0.016(3) -0.017(3)
C251 0.113(6) 0.068(5) 0.174(8) 0.005(5) -0.086(6) -0.028(4)
C252 0.074(4) 0.072(4) 0.102(5) -0.008(4) -0.043(4) -0.017(3)
C270 0.076(5) 0.092(5) 0.091(5) -0.037(4) 0.022(4) -0.035(4)
C271 0.135(7) 0.086(6) 0.125(7) 0.007(5) 0.037(6) -0.023(5)
C272 0.079(6) 0.136(8) 0.209(11) 0.048(7) 0.063(6) 0.021(6)
C290 0.042(3) 0.058(3) 0.068(4) -0.016(3) -0.018(3) -0.016(3)
C291 0.074(4) 0.073(4) 0.081(4) -0.013(3) -0.035(3) -0.025(3)
C292 0.059(4) 0.065(4) 0.089(5) -0.014(3) -0.032(3) -0.011(3)
C540 0.076(4) 0.112(5) 0.051(4) -0.039(4) -0.002(3) -0.032(4)
C541 0.066(5) 0.144(8) 0.180(9) 0.050(7) -0.004(6) -0.024(5)
C542 0.387(19) 0.150(9) 0.205(12) 0.040(8) -0.220(14) -0.120(11)
C560 0.082(6) 0.086(6) 0.376(18) -0.100(9) 0.090(9) -0.029(5)
C561 0.131(9) 0.215(13) 0.44(2) -0.257(16) -0.143(12) 0.094(9)
C562 0.094(7) 0.103(7) 0.335(18) 0.009(9) 0.067(9) 0.024(6)
C580 0.123(7) 0.114(7) 0.090(6) -0.009(5) -0.065(6) 0.045(6)
C581 0.39(2) 0.349(19) 0.090(8) -0.052(10) 0.021(11) -0.289(18)
C582 0.40(2) 0.50(3) 0.089(8) -0.017(12) -0.020(11) -0.37(2)
O300 0.120(5) 0.106(4) 0.173(6) 0.024(4) -0.073(5) -0.033(4)
C303 0.158(10) 0.110(7) 0.202(12) -0.059(7) -0.097(9) 0.030(7)
C302 0.151(10) 0.107(8) 0.261(16) -0.042(9) -0.058(10) -0.025(7)
C304 0.162(11) 0.175(11) 0.241(14) -0.039(10) -0.102(11) -0.051(10)
C301 0.184(13) 0.303(18) 0.211(14) -0.155(14) -0.049(11) 0.130(13)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Mo1 O3 2.100(3) 2_766 ?
Mo1 O1 2.100(3) . ?
Mo1 O4 2.106(3) . ?
Mo1 Mo1 2.1067(11) 2_766 ?
Mo1 O2 2.116(3) 2_766 ?
Mo2 O7 2.102(3) . ?
Mo2 O8 2.106(3) 2_675 ?
Mo2 Mo2 2.1079(10) 2_675 ?
Mo2 O6 2.109(3) 2_675 ?
Mo2 O5 2.115(3) . ?
N1 C7 1.396(5) . ?
N1 C16 1.431(6) . ?
N1 C10 1.441(6) . ?
N2 C22 1.140(6) . ?
N3 C36 1.392(5) . ?
N3 C45 1.437(5) . ?
N3 C39 1.443(5) . ?
N4 C51 1.134(6) . ?
O1 C1 1.278(5) . ?
O2 C1 1.283(5) . ?
O2 Mo1 2.116(3) 2_766 ?
O3 C23 1.259(5) . ?
O3 Mo1 2.100(3) 2_766 ?
O4 C23 1.282(5) . ?
O5 C30 1.266(5) . ?
O6 C30 1.272(5) . ?
O6 Mo2 2.109(3) 2_675 ?
O7 C52 1.266(6) . ?
O8 C52 1.284(5) . ?
O8 Mo2 2.106(3) 2_675 ?
O100 C101 1.376(8) . ?
O100 C104 1.395(7) . ?
O200 C201 1.435(6) . ?
O200 C204 1.437(6) . ?
C1 C2 1.481(6) . ?
C2 C3 1.356(6) . ?
C2 C22 1.437(7) . ?
C3 C4 1.445(6) . ?
C3 H3A 0.95 . ?
C4 C5 1.396(6) . ?
C4 C9 1.415(6) . ?
C5 C6 1.359(6) . ?
C5 H5A 0.95 . ?
C6 C7 1.406(6) . ?
C6 H6A 0.95 . ?
C7 C8 1.407(6) . ?
C8 C9 1.370(6) . ?
C8 H8A 0.95 . ?
C9 H9A 0.95 . ?
C10 C11 1.383(7) . ?
C10 C15 1.384(6) . ?
C11 C12 1.371(7) . ?
C11 H11A 0.95 . ?
C12 C13 1.365(7) . ?
C12 H12A 0.95 . ?
C13 C14 1.376(7) . ?
C13 H13A 0.95 . ?
C14 C15 1.371(6) . ?
C14 H14A 0.95 . ?
C15 H15A 0.95 . ?
C16 C21 1.377(7) . ?
C16 C17 1.405(7) . ?
C17 C18 1.365(7) . ?
C17 H17A 0.95 . ?
C18 C19 1.379(8) . ?
C18 H18A 0.95 . ?
C19 C20 1.393(8) . ?
C19 H19A 0.95 . ?
C20 C21 1.352(7) . ?
C20 H20A 0.95 . ?
C21 H21A 0.95 . ?
C23 C24 1.494(6) . ?
C24 C25 1.390(7) . ?
C24 C29 1.409(6) . ?
C25 C26 1.387(7) . ?
C25 C250 1.530(7) . ?
C26 C27 1.399(8) . ?
C26 H26A 0.95 . ?
C27 C28 1.380(8) . ?
C27 C270 1.539(8) . ?
C28 C29 1.388(7) . ?
C28 H28A 0.95 . ?
C29 C290 1.521(7) . ?
C30 C31 1.485(6) . ?
C31 C32 1.352(6) . ?
C31 C51 1.448(7) . ?
C32 C33 1.445(6) . ?
C32 H32A 0.95 . ?
C33 C34 1.398(6) . ?
C33 C38 1.404(6) . ?
C34 C35 1.376(6) . ?
C34 H34A 0.95 . ?
C35 C36 1.401(6) . ?
C35 H35A 0.95 . ?
C36 C37 1.398(6) . ?
C37 C38 1.370(6) . ?
C37 H37A 0.95 . ?
C38 H38A 0.95 . ?
C39 C40 1.370(6) . ?
C39 C44 1.391(6) . ?
C40 C41 1.375(7) . ?
C40 H40A 0.95 . ?
C41 C42 1.371(8) . ?
C41 H41A 0.95 . ?
C42 C43 1.367(8) . ?
C42 H42A 0.95 . ?
C43 C44 1.386(7) . ?
C43 H43A 0.95 . ?
C44 H44A 0.95 . ?
C45 C46 1.387(6) . ?
C45 C50 1.402(6) . ?
C46 C47 1.366(7) . ?
C46 H46A 0.95 . ?
C47 C48 1.397(7) . ?
C47 H47A 0.95 . ?
C48 C49 1.379(7) . ?
C48 H48A 0.95 . ?
C49 C50 1.372(6) . ?
C49 H49A 0.95 . ?
C50 H50A 0.95 . ?
C52 C53 1.501(7) . ?
C53 C58 1.391(8) . ?
C53 C54 1.396(7) . ?
C54 C55 1.394(8) . ?
C54 C540 1.491(8) . ?
C55 C56 1.379(11) . ?
C55 H55A 0.95 . ?
C56 C57 1.382(11) . ?
C56 C560 1.536(10) . ?
C57 C58 1.398(9) . ?
C57 H57A 0.95 . ?
C58 C580 1.513(10) . ?
C101 C102 1.517(10) . ?
C101 H10A 0.99 . ?
C101 H10B 0.99 . ?
C102 C103 1.530(12) . ?
C102 H10C 0.99 . ?
C102 H10D 0.99 . ?
C103 C104 1.433(10) . ?
C103 H10E 0.99 . ?
C103 H10F 0.99 . ?
C104 H10G 0.99 . ?
C104 H10H 0.99 . ?
C201 C202 1.491(9) . ?
C201 H20B 0.99 . ?
C201 H20C 0.99 . ?
C202 C203 1.491(9) . ?
C202 H20D 0.99 . ?
C202 H20E 0.99 . ?
C203 C204 1.477(8) . ?
C203 H20F 0.99 . ?
C203 H20G 0.99 . ?
C204 H20H 0.99 . ?
C204 H20I 0.99 . ?
C250 C252 1.492(8) . ?
C250 C251 1.500(8) . ?
C250 H25A 1 . ?
C251 H25B 0.98 . ?
C251 H25C 0.98 . ?
C251 H25D 0.98 . ?
C252 H25E 0.98 . ?
C252 H25F 0.98 . ?
C252 H25G 0.98 . ?
C270 C272 1.480(10) . ?
C270 C271 1.510(9) . ?
C270 H27A 1 . ?
C271 H27B 0.98 . ?
C271 H27C 0.98 . ?
C271 H27D 0.98 . ?
C272 H27E 0.98 . ?
C272 H27F 0.98 . ?
C272 H27G 0.98 . ?
C290 C292 1.526(7) . ?
C290 C291 1.532(7) . ?
C290 H29A 1 . ?
C291 H29B 0.98 . ?
C291 H29C 0.98 . ?
C291 H29D 0.98 . ?
C292 H29E 0.98 . ?
C292 H29F 0.98 . ?
C292 H29G 0.98 . ?
C540 C542 1.475(10) . ?
C540 C541 1.484(9) . ?
C540 H54A 1 . ?
C541 H54B 0.98 . ?
C541 H54C 0.98 . ?
C541 H54D 0.98 . ?
C542 H54E 0.98 . ?
C542 H54F 0.98 . ?
C542 H54G 0.98 . ?
C560 C561 1.299(13) . ?
C560 C562 1.399(13) . ?
C560 H56A 1 . ?
C561 H56B 0.98 . ?
C561 H56C 0.98 . ?
C561 H56D 0.98 . ?
C562 H56E 0.98 . ?
C562 H56F 0.98 . ?
C562 H56G 0.98 . ?
C580 C582 1.336(13) . ?
C580 C581 1.358(13) . ?
C580 H58A 1 . ?
C581 H58B 0.98 . ?
C581 H58C 0.98 . ?
C581 H58D 0.98 . ?
C582 H58E 0.98 . ?
C582 H58F 0.98 . ?
C582 H58G 0.98 . ?
O300 C304 1.416(11) . ?
O300 C301 1.418(12) . ?
C303 C302 1.503(14) . ?
C303 C304 1.512(14) . ?
C303 H30A 0.99 . ?
C303 H30B 0.99 . ?
C302 C301 1.442(13) . ?
C302 H30C 0.99 . ?
C302 H30D 0.99 . ?
C304 H30E 0.99 . ?
C304 H30F 0.99 . ?
C301 H30G 0.99 . ?
C301 H30H 0.99 . ?
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
O3 Mo1 O1 91.90(12) 2_766 . ?
O3 Mo1 O4 177.05(10) 2_766 . ?
O1 Mo1 O4 87.42(12) . . ?
O3 Mo1 Mo1 90.71(8) 2_766 2_766 ?
O1 Mo1 Mo1 92.06(8) . 2_766 ?
O4 Mo1 Mo1 92.18(8) . 2_766 ?
O3 Mo1 O2 88.47(12) 2_766 2_766 ?
O1 Mo1 O2 176.18(10) . 2_766 ?
O4 Mo1 O2 92.02(12) . 2_766 ?
Mo1 Mo1 O2 91.74(8) 2_766 2_766 ?
O7 Mo2 O8 176.48(12) . 2_675 ?
O7 Mo2 Mo2 92.62(9) . 2_675 ?
O8 Mo2 Mo2 90.90(9) 2_675 2_675 ?
O7 Mo2 O6 90.51(12) . 2_675 ?
O8 Mo2 O6 89.36(12) 2_675 2_675 ?
Mo2 Mo2 O6 91.89(9) 2_675 2_675 ?
O7 Mo2 O5 88.88(12) . . ?
O8 Mo2 O5 91.04(12) 2_675 . ?
Mo2 Mo2 O5 91.53(9) 2_675 . ?
O6 Mo2 O5 176.55(11) 2_675 . ?
C7 N1 C16 123.2(4) . . ?
C7 N1 C10 118.3(4) . . ?
C16 N1 C10 118.4(3) . . ?
C36 N3 C45 122.8(4) . . ?
C36 N3 C39 119.6(4) . . ?
C45 N3 C39 116.8(4) . . ?
C1 O1 Mo1 117.0(3) . . ?
C1 O2 Mo1 116.4(3) . 2_766 ?
C23 O3 Mo1 119.1(3) . 2_766 ?
C23 O4 Mo1 116.8(3) . . ?
C30 O5 Mo2 116.7(3) . . ?
C30 O6 Mo2 116.5(3) . 2_675 ?
C52 O7 Mo2 116.4(3) . . ?
C52 O8 Mo2 117.4(3) . 2_675 ?
C101 O100 C104 110.2(5) . . ?
C201 O200 C204 106.3(4) . . ?
O1 C1 O2 122.6(4) . . ?
O1 C1 C2 118.9(4) . . ?
O2 C1 C2 118.4(4) . . ?
C3 C2 C22 125.2(4) . . ?
C3 C2 C1 119.1(4) . . ?
C22 C2 C1 115.7(4) . . ?
C2 C3 C4 132.7(4) . . ?
C2 C3 H3A 113.6 . . ?
C4 C3 H3A 113.6 . . ?
C5 C4 C9 117.4(4) . . ?
C5 C4 C3 117.3(4) . . ?
C9 C4 C3 125.3(4) . . ?
C6 C5 C4 122.2(4) . . ?
C6 C5 H5A 118.9 . . ?
C4 C5 H5A 118.9 . . ?
C5 C6 C7 120.6(4) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
N1 C7 C6 120.2(4) . . ?
N1 C7 C8 121.8(4) . . ?
C6 C7 C8 118.0(4) . . ?
C9 C8 C7 121.0(4) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C4 120.7(4) . . ?
C8 C9 H9A 119.6 . . ?
C4 C9 H9A 119.6 . . ?
C11 C10 C15 119.7(4) . . ?
C11 C10 N1 120.9(4) . . ?
C15 C10 N1 119.3(4) . . ?
C12 C11 C10 120.0(5) . . ?
C12 C11 H11A 120 . . ?
C10 C11 H11A 120 . . ?
C13 C12 C11 120.3(5) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C14 120.0(5) . . ?
C12 C13 H13A 120 . . ?
C14 C13 H13A 120 . . ?
C15 C14 C13 120.5(5) . . ?
C15 C14 H14A 119.8 . . ?
C13 C14 H14A 119.8 . . ?
C14 C15 C10 119.5(5) . . ?
C14 C15 H15A 120.2 . . ?
C10 C15 H15A 120.3 . . ?
C21 C16 C17 118.2(5) . . ?
C21 C16 N1 122.7(4) . . ?
C17 C16 N1 119.1(4) . . ?
C18 C17 C16 120.4(5) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C19 120.9(6) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C20 118.3(6) . . ?
C18 C19 H19A 120.9 . . ?
C20 C19 H19A 120.8 . . ?
C21 C20 C19 121.2(6) . . ?
C21 C20 H20A 119.4 . . ?
C19 C20 H20A 119.4 . . ?
C20 C21 C16 121.1(5) . . ?
C20 C21 H21A 119.5 . . ?
C16 C21 H21A 119.5 . . ?
N2 C22 C2 179.4(7) . . ?
O3 C23 O4 121.1(4) . . ?
O3 C23 C24 119.2(4) . . ?
O4 C23 C24 119.6(4) . . ?
C25 C24 C29 120.6(5) . . ?
C25 C24 C23 120.5(4) . . ?
C29 C24 C23 118.9(4) . . ?
C26 C25 C24 118.8(5) . . ?
C26 C25 C250 119.2(5) . . ?
C24 C25 C250 122.0(5) . . ?
C25 C26 C27 122.1(5) . . ?
C25 C26 H26A 118.9 . . ?
C27 C26 H26A 118.9 . . ?
C28 C27 C26 117.7(5) . . ?
C28 C27 C270 121.8(6) . . ?
C26 C27 C270 120.5(6) . . ?
C27 C28 C29 122.3(5) . . ?
C27 C28 H28A 118.8 . . ?
C29 C28 H28A 118.8 . . ?
C28 C29 C24 118.5(5) . . ?
C28 C29 C290 119.8(5) . . ?
C24 C29 C290 121.7(5) . . ?
O5 C30 O6 123.3(4) . . ?
O5 C30 C31 118.1(4) . . ?
O6 C30 C31 118.5(4) . . ?
C32 C31 C51 123.7(4) . . ?
C32 C31 C30 120.8(4) . . ?
C51 C31 C30 115.5(4) . . ?
C31 C32 C33 132.6(4) . . ?
C31 C32 H32A 113.7 . . ?
C33 C32 H32A 113.7 . . ?
C34 C33 C38 117.3(4) . . ?
C34 C33 C32 117.6(4) . . ?
C38 C33 C32 125.1(4) . . ?
C35 C34 C33 122.2(4) . . ?
C35 C34 H34A 118.9 . . ?
C33 C34 H34A 118.9 . . ?
C34 C35 C36 120.2(4) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
N3 C36 C37 122.7(4) . . ?
N3 C36 C35 119.6(4) . . ?
C37 C36 C35 117.7(4) . . ?
C38 C37 C36 121.9(4) . . ?
C38 C37 H37A 119 . . ?
C36 C37 H37A 119 . . ?
C37 C38 C33 120.7(4) . . ?
C37 C38 H38A 119.7 . . ?
C33 C38 H38A 119.7 . . ?
C40 C39 C44 119.8(4) . . ?
C40 C39 N3 121.3(4) . . ?
C44 C39 N3 118.8(4) . . ?
C39 C40 C41 119.7(5) . . ?
C39 C40 H40A 120.1 . . ?
C41 C40 H40A 120.1 . . ?
C42 C41 C40 120.8(5) . . ?
C42 C41 H41A 119.6 . . ?
C40 C41 H41A 119.6 . . ?
C43 C42 C41 120.1(5) . . ?
C43 C42 H42A 119.9 . . ?
C41 C42 H42A 119.9 . . ?
C42 C43 C44 119.7(6) . . ?
C42 C43 H43A 120.1 . . ?
C44 C43 H43A 120.1 . . ?
C43 C44 C39 119.8(5) . . ?
C43 C44 H44A 120.1 . . ?
C39 C44 H44A 120.1 . . ?
C46 C45 C50 119.7(4) . . ?
C46 C45 N3 119.6(4) . . ?
C50 C45 N3 120.6(4) . . ?
C47 C46 C45 120.2(5) . . ?
C47 C46 H46A 119.9 . . ?
C45 C46 H46A 119.9 . . ?
C46 C47 C48 120.4(5) . . ?
C46 C47 H47A 119.8 . . ?
C48 C47 H47A 119.8 . . ?
C49 C48 C47 119.4(5) . . ?
C49 C48 H48A 120.3 . . ?
C47 C48 H48A 120.3 . . ?
C50 C49 C48 120.8(5) . . ?
C50 C49 H49A 119.6 . . ?
C48 C49 H49A 119.6 . . ?
C49 C50 C45 119.5(4) . . ?
C49 C50 H50A 120.2 . . ?
C45 C50 H50A 120.2 . . ?
N4 C51 C31 179.2(6) . . ?
O7 C52 O8 122.6(4) . . ?
O7 C52 C53 119.9(4) . . ?
O8 C52 C53 117.5(4) . . ?
C58 C53 C54 122.6(5) . . ?
C58 C53 C52 119.6(5) . . ?
C54 C53 C52 117.8(5) . . ?
C55 C54 C53 117.2(6) . . ?
C55 C54 C540 121.9(6) . . ?
C53 C54 C540 120.9(5) . . ?
C56 C55 C54 122.4(7) . . ?
C56 C55 H55A 118.8 . . ?
C54 C55 H55A 118.8 . . ?
C55 C56 C57 118.4(6) . . ?
C55 C56 C560 120.4(10) . . ?
C57 C56 C560 121.3(10) . . ?
C56 C57 C58 122.2(7) . . ?
C56 C57 H57A 118.9 . . ?
C58 C57 H57A 118.9 . . ?
C53 C58 C57 117.2(6) . . ?
C53 C58 C580 120.7(5) . . ?
C57 C58 C580 122.1(6) . . ?
O100 C101 C102 107.4(7) . . ?
O100 C101 H10A 110.2 . . ?
C102 C101 H10A 110.2 . . ?
O100 C101 H10B 110.2 . . ?
C102 C101 H10B 110.2 . . ?
H10A C101 H10B 108.5 . . ?
C101 C102 C103 105.0(7) . . ?
C101 C102 H10C 110.7 . . ?
C103 C102 H10C 110.7 . . ?
C101 C102 H10D 110.7 . . ?
C103 C102 H10D 110.7 . . ?
H10C C102 H10D 108.8 . . ?
C104 C103 C102 102.9(8) . . ?
C104 C103 H10E 111.2 . . ?
C102 C103 H10E 111.2 . . ?
C104 C103 H10F 111.2 . . ?
C102 C103 H10F 111.2 . . ?
H10E C103 H10F 109.1 . . ?
O100 C104 C103 112.3(6) . . ?
O100 C104 H10G 109.2 . . ?
C103 C104 H10G 109.2 . . ?
O100 C104 H10H 109.2 . . ?
C103 C104 H10H 109.2 . . ?
H10G C104 H10H 107.9 . . ?
O200 C201 C202 105.7(5) . . ?
O200 C201 H20B 110.6 . . ?
C202 C201 H20B 110.6 . . ?
O200 C201 H20C 110.6 . . ?
C202 C201 H20C 110.6 . . ?
H20B C201 H20C 108.7 . . ?
C203 C202 C201 103.9(5) . . ?
C203 C202 H20D 111 . . ?
C201 C202 H20D 111 . . ?
C203 C202 H20E 111 . . ?
C201 C202 H20E 111 . . ?
H20D C202 H20E 109 . . ?
C204 C203 C202 105.9(6) . . ?
C204 C203 H20F 110.6 . . ?
C202 C203 H20F 110.6 . . ?
C204 C203 H20G 110.6 . . ?
C202 C203 H20G 110.6 . . ?
H20F C203 H20G 108.7 . . ?
O200 C204 C203 108.2(5) . . ?
O200 C204 H20H 110.1 . . ?
C203 C204 H20H 110.1 . . ?
O200 C204 H20I 110.1 . . ?
C203 C204 H20I 110.1 . . ?
H20H C204 H20I 108.4 . . ?
C252 C250 C251 111.3(5) . . ?
C252 C250 C25 113.5(5) . . ?
C251 C250 C25 111.4(5) . . ?
C252 C250 H25A 106.7 . . ?
C251 C250 H25A 106.7 . . ?
C25 C250 H25A 106.7 . . ?
C250 C251 H25B 109.5 . . ?
C250 C251 H25C 109.5 . . ?
H25B C251 H25C 109.5 . . ?
C250 C251 H25D 109.5 . . ?
H25B C251 H25D 109.5 . . ?
H25C C251 H25D 109.5 . . ?
C250 C252 H25E 109.5 . . ?
C250 C252 H25F 109.5 . . ?
H25E C252 H25F 109.5 . . ?
C250 C252 H25G 109.5 . . ?
H25E C252 H25G 109.5 . . ?
H25F C252 H25G 109.5 . . ?
C272 C270 C271 110.0(7) . . ?
C272 C270 C27 112.3(6) . . ?
C271 C270 C27 111.9(5) . . ?
C272 C270 H27A 107.4 . . ?
C271 C270 H27A 107.5 . . ?
C27 C270 H27A 107.5 . . ?
C270 C271 H27B 109.5 . . ?
C270 C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C270 C271 H27D 109.5 . . ?
H27B C271 H27D 109.5 . . ?
H27C C271 H27D 109.5 . . ?
C270 C272 H27E 109.5 . . ?
C270 C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C270 C272 H27G 109.5 . . ?
H27E C272 H27G 109.5 . . ?
H27F C272 H27G 109.5 . . ?
C29 C290 C292 110.6(4) . . ?
C29 C290 C291 113.0(4) . . ?
C292 C290 C291 109.4(4) . . ?
C29 C290 H29A 107.9 . . ?
C292 C290 H29A 107.9 . . ?
C291 C290 H29A 107.9 . . ?
C290 C291 H29B 109.5 . . ?
C290 C291 H29C 109.5 . . ?
H29B C291 H29C 109.5 . . ?
C290 C291 H29D 109.5 . . ?
H29B C291 H29D 109.5 . . ?
H29C C291 H29D 109.5 . . ?
C290 C292 H29E 109.5 . . ?
C290 C292 H29F 109.5 . . ?
H29E C292 H29F 109.5 . . ?
C290 C292 H29G 109.5 . . ?
H29E C292 H29G 109.5 . . ?
H29F C292 H29G 109.5 . . ?
C542 C540 C541 114.7(8) . . ?
C542 C540 C54 114.1(6) . . ?
C541 C540 C54 112.8(6) . . ?
C542 C540 H54A 104.6 . . ?
C541 C540 H54A 104.6 . . ?
C54 C540 H54A 104.6 . . ?
C540 C541 H54B 109.5 . . ?
C540 C541 H54C 109.5 . . ?
H54B C541 H54C 109.5 . . ?
C540 C541 H54D 109.5 . . ?
H54B C541 H54D 109.5 . . ?
H54C C541 H54D 109.5 . . ?
C540 C542 H54E 109.5 . . ?
C540 C542 H54F 109.5 . . ?
H54E C542 H54F 109.5 . . ?
C540 C542 H54G 109.5 . . ?
H54E C542 H54G 109.5 . . ?
H54F C542 H54G 109.5 . . ?
C561 C560 C562 126.2(9) . . ?
C561 C560 C56 117.2(8) . . ?
C562 C560 C56 112.0(8) . . ?
C561 C560 H56A 97.1 . . ?
C562 C560 H56A 97.1 . . ?
C56 C560 H56A 97.1 . . ?
C560 C561 H56B 109.5 . . ?
C560 C561 H56C 109.5 . . ?
H56B C561 H56C 109.5 . . ?
C560 C561 H56D 109.5 . . ?
H56B C561 H56D 109.5 . . ?
H56C C561 H56D 109.5 . . ?
C560 C562 H56E 109.5 . . ?
C560 C562 H56F 109.5 . . ?
H56E C562 H56F 109.5 . . ?
C560 C562 H56G 109.5 . . ?
H56E C562 H56G 109.5 . . ?
H56F C562 H56G 109.5 . . ?
C582 C580 C581 111.3(9) . . ?
C582 C580 C58 116.4(10) . . ?
C581 C580 C58 115.7(10) . . ?
C582 C580 H58A 103.8 . . ?
C581 C580 H58A 103.8 . . ?
C58 C580 H58A 103.8 . . ?
C580 C581 H58B 109.5 . . ?
C580 C581 H58C 109.5 . . ?
H58B C581 H58C 109.5 . . ?
C580 C581 H58D 109.5 . . ?
H58B C581 H58D 109.5 . . ?
H58C C581 H58D 109.5 . . ?
C580 C582 H58E 109.5 . . ?
C580 C582 H58F 109.5 . . ?
H58E C582 H58F 109.5 . . ?
C580 C582 H58G 109.5 . . ?
H58E C582 H58G 109.5 . . ?
H58F C582 H58G 109.5 . . ?
C304 O300 C301 106.2(9) . . ?
C302 C303 C304 104.8(9) . . ?
C302 C303 H30A 110.8 . . ?
C304 C303 H30A 110.8 . . ?
C302 C303 H30B 110.8 . . ?
C304 C303 H30B 110.8 . . ?
H30A C303 H30B 108.9 . . ?
C301 C302 C303 103.6(10) . . ?
C301 C302 H30C 111 . . ?
C303 C302 H30C 111 . . ?
C301 C302 H30D 111.1 . . ?
C303 C302 H30D 111 . . ?
H30C C302 H30D 109 . . ?
O300 C304 C303 109.3(10) . . ?
O300 C304 H30E 109.8 . . ?
C303 C304 H30E 109.8 . . ?
O300 C304 H30F 109.8 . . ?
C303 C304 H30F 109.8 . . ?
H30E C304 H30F 108.3 . . ?
O300 C301 C302 112.2(12) . . ?
O300 C301 H30G 109.2 . . ?
C302 C301 H30G 109.2 . . ?
O300 C301 H30H 109.2 . . ?
C302 C301 H30H 109.1 . . ?
H30G C301 H30H 107.9 . . ?
# END of CIF