# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1863

 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 1999-07-30 at 14:04:03
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1beta3
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : lkmo2n dreduc struct psi_scan
 
#
#     CCDC ELECTRONIC DATA DEPOSITION FORM (CIF)
#
#     This electronic data deposition form can be used:
#
#     (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or
#     (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC
#
#     A comprehensive archive of CIF resources is maintained by the IUCr
#     at its Chester office. This can be accessed
#     by anonymous ftp to ftp.iucr.org
#     or via the WWW at http://www.iucr.org/cif/home.html
#     If data items in this form are not available or not applicable
#     then ignore these items
#     A few items specific to CCDC input are indicated by _ccdc_
#
#     Submission and help information is provided at the end of this form
#-------------------------------------------------------------------------
#1    Global data block identification for start of deposition
 
data_global
 
#
#-------------------------------------------------------------------------
#2    Person making the deposition
#
_publ_contact_author               'Sullivan A. C.'
_publ_contact_author_email          A.C.Sullivan@qmw.ac.uk
 
#-------------------------------------------------------------------------
#3    Publication details
#
#     Provide these details if the structure has been published,
#     accepted or submitted for publication
#
#     The CCDC journal deposition number, eg. 182/357,
#     should be included only if it has been assigned by the journal
#
loop_
_publ_author_name
 
'Sullivan A. C.'
 
_journal_name_full                 'private communication'
_journal_volume                    ?
_journal_page_first                ?
_journal_page_last                 ?
_journal_year                      ?
_ccdc_journal_depnumber            ?
#
#-------------------------------------------------------------------------
#4    Chemical and physical data
#
#     Note that the units for melting point are Kelvin
#     The compound_id is the identifier for the compound in the published
#       paper, eg. 4a, II, etc.
#     Provide a brief description of any significant biological activity,
#       eg. antimalarial activity
#     If the compound exhibits polymorphism provide brief details,
#       eg. monoclinic form, low-temperature phase, etc.
#     For chemdiag  leave blank - no longer necessary
 
_ccdc_compound_id                  ?
_ccdc_biological_activity          ?
_ccdc_polymorph                    ?
 
_ccdc_chemdiag_type                ?
_ccdc_chemdiag_records
;
?
;
#
#-------------------------------------------------------------------------
#5    Other data relating to the structure determination and refinement
#
#     Record the radiation type if not X-rays, eg. neutron
#     Record the temperature of the data collection (Kelvin)
#       if not room-temperature
#     Record R_squared if this is the only reliability factor given by
#       your refinement program
#     Describe briefly any disorder, eg. t-Butyl C31-33 disordered over
#       two sites with occupancies 0.6 and 0.4
#     Under ccdc_comments record any other important information
 
_ccdc_temp_data_collection          220 
_ccdc_ls_R_squared                  ?
_ccdc_disorder                      ?
_ccdc_comments
;
?
;
#-------------------------------------------------------------------------
#6    Include your "standard" CIF file here
#     It should contain the following data items:
#       unit cell parameters and volume, z value, space group symbol,
#       R-factor(s), atomic coordinates with standard deviations,
#       occupancy factors, bond lengths and bond angles
#     Other data items may be present but will not necessarily be
#       included in the Cambridge Structural Database
#
#     Do NOT include structure factors
#
#
#-------------------------------------------------------------------------
#SUBMISSION INFORMATION
#
#     For a journal send the form to the address specified by the journal
#
#     For a private communication to the CCDC send the form to the address
#       deposit@ccdc.cam.ac.uk
#
#     For up-to-date information on deposition procedures, check the website
#       http://www.ccdc.cam.ac.uk/
 
data_lkmo2n
 
_audit_creation_date            1999-07-30T14:04:03-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C92 H120 N4 O6 SI4 MO2'
_chemical_formula_structural            'C92 H120 N4 O6 SI4 MO2'
_chemical_formula_sum                   'C102 H114 Mo2 N4 O6 Si4'
_chemical_formula_weight                1796.21
_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                          17.106(6)
_cell_length_b                          13.531(8)
_cell_length_c                          13.128(7)
_cell_angle_alpha                       116.83(5)
_cell_angle_beta                        112.58(3)
_cell_angle_gamma                       90.83(5)
_cell_volume                            2438(2)
_cell_formula_units_Z                   1
_cell_measurement_temperature           220(2)
_cell_measurement_reflns_used           25
_cell_measurement_theta_min             0
_cell_measurement_theta_max             0
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              'diamond plate'
_exptl_crystal_colour                   'tranaparent orange'
_exptl_crystal_size_max                 0.375
_exptl_crystal_size_mid                 0.275
_exptl_crystal_size_min                 0.125
_exptl_crystal_density_diffrn           1.224
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    942
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.359
_exptl_absorpt_factor_muR               0.12
_exptl_absorpt_correction_type          psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_absorpt_correction_T_min         0.7802
_exptl_absorpt_correction_T_max         0.8849
_exptl_absorpt_correction_T_ave         0.833
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             220(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_measurement_device              'Enraf Nonius CAD4'
_diffrn_measurement_method              'non-profiled omega/2theta scans'
_diffrn_standards_number                2
_diffrn_standards_interval_time         60
_diffrn_standards_decay_%               4
_diffrn_standards_decay_corr_max        1.477
_diffrn_standards_decay_corr_min        0.996
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
9 1 -4
-3 4 -3
 
_diffrn_reflns_number                   8869
_diffrn_reflns_av_R_equivalents         0.0573
_diffrn_reflns_av_sigmaI/netI           0.1035
_diffrn_reflns_limit_h_min              0
_diffrn_reflns_limit_h_max              20
_diffrn_reflns_limit_k_min              -16
_diffrn_reflns_limit_k_max              16
_diffrn_reflns_limit_l_min              -15
_diffrn_reflns_limit_l_max              14
_diffrn_reflns_theta_min                1.73
_diffrn_reflns_theta_max                25
_diffrn_reflns_theta_full               25
_diffrn_measured_fraction_theta_full
                                        0.997
_diffrn_measured_fraction_theta_max
                                        0.997
_reflns_number_total                    8552
_reflns_number_gt                       5614
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'CAD4/PC (Enraf Nonius, 1992)'
_computing_cell_refinement              'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_reduction               'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1997)'
 
#----------------------------------------------------------------------------#
#                   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^ > 2sigma(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
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                8552
_refine_ls_number_parameters            496
_refine_ls_number_restraints            2
_refine_ls_R_factor_all                 0.1229
_refine_ls_R_factor_gt                  0.0559
_refine_ls_wR_factor_ref                0.1564
_refine_ls_wR_factor_gt                 0.134
_refine_ls_goodness_of_fit_ref          1.022
_refine_ls_restrained_S_all             1.024
_refine_ls_shift/su_max                 0.176
_refine_ls_shift/su_mean                0.005
_refine_diff_density_max                0.872
_refine_diff_density_min                -0.552
_refine_diff_density_rms                0.097
 
#----------------------------------------------------------------------------#
#                   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'
Si Si 0.0817 0.0704 '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 0.80683(3) 0.44347(4) -0.07752(4) 0.02527(14) Uani 1 1 d . . .
Si1 Si 0.92328(9) 0.71622(12) 0.17706(13) 0.0295(3) Uani 1 1 d . . .
Si2 Si 1.07597(9) 0.76922(12) 0.11382(14) 0.0292(3) Uani 1 1 d . . .
O1 O 0.8732(2) 0.5891(3) 0.0572(3) 0.0408(9) Uani 1 1 d . . .
O2 O 1.0085(2) 0.7582(3) 0.1687(3) 0.0395(9) Uani 1 1 d . . .
O3 O 0.8744(2) 0.3335(3) -0.0936(4) 0.0491(10) Uani 1 1 d . . .
N1 N 0.7644(3) 0.4483(3) -0.2188(4) 0.0319(10) Uani 1 1 d . . .
N2 N 0.7229(3) 0.4053(4) -0.0492(4) 0.0344(10) Uani 1 1 d . . .
C1 C 0.7052(3) 0.4372(5) -0.3340(5) 0.0326(12) Uani 1 1 d . . .
C2 C 0.6758(3) 0.5343(5) -0.3339(5) 0.0348(12) Uani 1 1 d . . .
C3 C 0.6185(4) 0.5228(6) -0.4500(6) 0.0522(16) Uani 1 1 d . . .
H3 H 0.5971 0.5846 -0.4534 0.059(11) Uiso 1 1 calc R . .
C4 C 0.5933(4) 0.4190(7) -0.5606(6) 0.0605(19) Uani 1 1 d . . .
H4 H 0.5553 0.4126 -0.6375 0.059(11) Uiso 1 1 calc R . .
C5 C 0.6225(4) 0.3265(6) -0.5598(5) 0.0528(17) Uani 1 1 d . . .
H5 H 0.6043 0.2585 -0.6359 0.059(11) Uiso 1 1 calc R . .
C6 C 0.6796(3) 0.3316(5) -0.4464(5) 0.0388(13) Uani 1 1 d . . .
C7 C 0.7054(4) 0.6470(5) -0.2101(5) 0.0396(13) Uani 1 1 d . . .
H7 H 0.7663 0.6544 -0.1568 0.047(16) Uiso 1 1 calc R . .
C8 C 0.7006(5) 0.7505(6) -0.2299(7) 0.066(2) Uani 1 1 d . . .
H8A H 0.7269 0.8189 -0.1489 0.084(14) Uiso 1 1 calc R . .
H8B H 0.6408 0.7499 -0.2742 0.084(14) Uiso 1 1 calc R . .
H8C H 0.731 0.7474 -0.279 0.084(14) Uiso 1 1 calc R . .
C9 C 0.6528(4) 0.6467(5) -0.1384(6) 0.0503(16) Uani 1 1 d . . .
H9A H 0.5925 0.6391 -0.1887 0.073(12) Uiso 1 1 calc R . .
H9B H 0.6738 0.7167 -0.0592 0.073(12) Uiso 1 1 calc R . .
H9C H 0.659 0.584 -0.1223 0.073(12) Uiso 1 1 calc R . .
C10 C 0.7154(4) 0.2308(5) -0.4437(5) 0.0448(14) Uani 1 1 d . . .
H10 H 0.7231 0.2349 -0.3638 0.036(14) Uiso 1 1 calc R . .
C11 C 0.6557(5) 0.1144(6) -0.5523(7) 0.069(2) Uani 1 1 d . . .
H11A H 0.679 0.0553 -0.538 0.088(15) Uiso 1 1 calc R . .
H11B H 0.652 0.1041 -0.6315 0.088(15) Uiso 1 1 calc R . .
H11C H 0.5987 0.1112 -0.5553 0.088(15) Uiso 1 1 calc R . .
C12 C 0.8047(4) 0.2416(7) -0.4413(8) 0.069(2) Uani 1 1 d . . .
H12A H 0.8294 0.1806 -0.4336 0.067(12) Uiso 1 1 calc R . .
H12B H 0.8418 0.3131 -0.3702 0.067(12) Uiso 1 1 calc R . .
H12C H 0.7994 0.238 -0.5185 0.067(12) Uiso 1 1 calc R . .
C13 C 0.6458(3) 0.3871(4) -0.0390(5) 0.0354(12) Uani 1 1 d . . .
C14 C 0.5658(4) 0.3307(5) -0.1475(6) 0.0427(14) Uani 1 1 d . . .
C15 C 0.4919(4) 0.3188(6) -0.1297(7) 0.0590(18) Uani 1 1 d . . .
H15 H 0.4382 0.2821 -0.2002 0.089(15) Uiso 1 1 calc R . .
C16 C 0.4964(5) 0.3603(7) -0.0095(7) 0.071(2) Uani 1 1 d . . .
H16 H 0.446 0.3523 0.0003 0.089(15) Uiso 1 1 calc R . .
C17 C 0.5757(5) 0.4135(6) 0.0957(7) 0.0628(19) Uani 1 1 d . . .
H17 H 0.5782 0.4406 0.1761 0.089(15) Uiso 1 1 calc R . .
C18 C 0.6521(4) 0.4274(5) 0.0841(6) 0.0495(15) Uani 1 1 d . . .
C19 C 0.5578(4) 0.2810(5) -0.2812(6) 0.0467(15) Uani 1 1 d . . .
H19 H 0.6162 0.2962 -0.2745 0.07(2) Uiso 1 1 calc R . .
C20 C 0.5235(5) 0.1520(6) -0.3549(7) 0.075(2) Uani 1 1 d . . .
H20A H 0.5619 0.1186 -0.3109 0.103(17) Uiso 1 1 calc R . .
H20B H 0.5207 0.1219 -0.4382 0.103(17) Uiso 1 1 calc R . .
H20C H 0.4665 0.1345 -0.3619 0.103(17) Uiso 1 1 calc R . .
C21 C 0.5019(4) 0.3362(6) -0.3514(6) 0.0589(18) Uani 1 1 d . . .
H21A H 0.4991 0.3033 -0.4349 0.057(11) Uiso 1 1 calc R . .
H21B H 0.5268 0.4164 -0.3059 0.057(11) Uiso 1 1 calc R . .
H21C H 0.4444 0.324 -0.3579 0.057(11) Uiso 1 1 calc R . .
C22 C 0.7400(4) 0.4806(6) 0.1994(6) 0.0588(18) Uani 1 1 d . . .
H22 H 0.7779 0.5152 0.1784 0.07(2) Uiso 1 1 calc R . .
C23 C 0.7797(6) 0.3909(8) 0.2222(9) 0.104(3) Uani 1 1 d . . .
H23A H 0.8367 0.425 0.2918 0.084(14) Uiso 1 1 calc R . .
H23B H 0.7839 0.3358 0.1473 0.084(14) Uiso 1 1 calc R . .
H23C H 0.7441 0.3541 0.2423 0.084(14) Uiso 1 1 calc R . .
C24 C 0.7382(6) 0.5754(8) 0.3193(7) 0.096(3) Uani 1 1 d . . .
H24A H 0.7054 0.6262 0.2989 0.105(17) Uiso 1 1 calc R . .
H24B H 0.7966 0.6167 0.3815 0.105(17) Uiso 1 1 calc R . .
H24C H 0.7115 0.5428 0.3529 0.105(17) Uiso 1 1 calc R . .
C25 C 0.9602(2) 0.7108(3) 0.3278(3) 0.0402(13) Uani 1 1 d G . .
C26 C 0.9823(3) 0.8106(3) 0.4418(4) 0.0572(17) Uani 1 1 d G . .
H26 H 0.9731 0.8781 0.4418 0.085(11) Uiso 1 1 calc R . .
C27 C 1.0182(3) 0.8094(4) 0.5557(3) 0.082(3) Uani 1 1 d G . .
H27 H 1.0329 0.8762 0.632 0.085(11) Uiso 1 1 calc R . .
C28 C 1.0319(3) 0.7084(5) 0.5557(4) 0.084(3) Uani 1 1 d G . .
H28 H 1.0559 0.7076 0.632 0.085(11) Uiso 1 1 calc R . .
C29 C 1.0098(3) 0.6086(4) 0.4418(5) 0.068(2) Uani 1 1 d G . .
H29 H 1.019 0.541 0.4418 0.085(11) Uiso 1 1 calc R . .
C30 C 0.9740(3) 0.6098(3) 0.3278(4) 0.0509(16) Uani 1 1 d G . .
H30 H 0.9592 0.543 0.2515 0.085(11) Uiso 1 1 calc R . .
C31 C 0.8525(2) 0.8207(3) 0.1750(4) 0.0426(14) Uani 1 1 d G . .
C32 C 0.8614(3) 0.8931(4) 0.1296(4) 0.0542(17) Uani 1 1 d G . .
H32 H 0.903 0.8903 0.0995 0.088(11) Uiso 1 1 calc R . .
C33 C 0.8083(3) 0.9698(4) 0.1292(5) 0.075(2) Uani 1 1 d G . .
H33 H 0.8143 1.0183 0.0988 0.088(11) Uiso 1 1 calc R . .
C34 C 0.7462(3) 0.9740(4) 0.1741(5) 0.093(3) Uani 1 1 d G . .
H34 H 0.7106 1.0253 0.1738 0.088(11) Uiso 1 1 calc R . .
C35 C 0.7373(3) 0.9016(5) 0.2195(5) 0.093(3) Uani 1 1 d G . .
H35 H 0.6957 0.9044 0.2496 0.088(11) Uiso 1 1 calc R . .
C36 C 0.7904(3) 0.8249(4) 0.2199(4) 0.065(2) Uani 1 1 d G . .
H36 H 0.7844 0.7764 0.2503 0.088(11) Uiso 1 1 calc R . .
C37 C 1.1559(2) 0.9097(3) 0.2371(3) 0.0415(14) Uani 1 1 d G . .
C38 C 1.1382(2) 0.9879(3) 0.3346(4) 0.0512(16) Uani 1 1 d G . .
H38 H 1.087 0.9709 0.3387 0.087(11) Uiso 1 1 calc R . .
C39 C 1.1971(3) 1.0915(3) 0.4258(3) 0.072(2) Uani 1 1 d G . .
H39 H 1.1853 1.1439 0.4911 0.087(11) Uiso 1 1 calc R . .
C40 C 1.2736(3) 1.1170(3) 0.4197(4) 0.084(3) Uani 1 1 d G . .
H40 H 1.313 1.1863 0.4808 0.087(11) Uiso 1 1 calc R . .
C41 C 1.2913(2) 1.0388(4) 0.3222(5) 0.081(3) Uani 1 1 d G . .
H41 H 1.3425 1.0558 0.3181 0.087(11) Uiso 1 1 calc R . .
C42 C 1.2324(3) 0.9351(4) 0.2309(4) 0.0636(19) Uani 1 1 d G . .
H42 H 1.2442 0.8828 0.1657 0.087(11) Uiso 1 1 calc R . .
C43 C 1.0123(2) 0.7566(3) -0.0450(3) 0.0342(12) Uani 1 1 d G . .
C44 C 1.0169(3) 0.8489(3) -0.0645(3) 0.0560(17) Uani 1 1 d G . .
H44 H 1.055 0.918 0.0011 0.074(10) Uiso 1 1 calc R . .
C45 C 0.9647(3) 0.8378(3) -0.1821(4) 0.076(2) Uani 1 1 d G . .
H45 H 0.9678 0.8995 -0.1952 0.074(10) Uiso 1 1 calc R . .
C46 C 0.9079(3) 0.7344(4) -0.2802(3) 0.075(2) Uani 1 1 d G . .
H46 H 0.873 0.727 -0.3589 0.074(10) Uiso 1 1 calc R . .
C47 C 0.9033(2) 0.6422(3) -0.2606(3) 0.0600(18) Uani 1 1 d G . .
H47 H 0.8653 0.573 -0.3262 0.074(10) Uiso 1 1 calc R . .
C48 C 0.9555(3) 0.6533(3) -0.1430(4) 0.0485(15) Uani 1 1 d G . .
H48 H 0.9524 0.5916 -0.1299 0.074(10) Uiso 1 1 calc R . .
C49 C 0.5136(10) 1.0928(14) 0.0387(14) 0.173(6) Uiso 1 1 d D . .
H49 H 0.5165 1.1706 0.0761 0.13(2) Uiso 1 1 calc R . .
C50 C 0.5646(13) 1.0602(19) -0.0551(18) 0.234(9) Uiso 1 1 d D . .
H50 H 0.5973 1.0965 -0.0761 0.13(2) Uiso 1 1 calc R . .
C51 C 0.5344(12) 0.9574(19) -0.0834(19) 0.228(8) Uiso 1 1 d D . .
H51 H 0.5457 0.9022 -0.1473 0.13(2) 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 0.0247(2) 0.0214(2) 0.0236(2) 0.00800(18) 0.00876(17) 0.00376(16)
Si1 0.0295(8) 0.0246(7) 0.0255(7) 0.0063(6) 0.0114(6) 0.0007(6)
Si2 0.0289(7) 0.0248(7) 0.0346(8) 0.0144(6) 0.0148(6) 0.0066(6)
O1 0.040(2) 0.029(2) 0.030(2) 0.0044(17) 0.0064(17) -0.0015(17)
O2 0.035(2) 0.042(2) 0.044(2) 0.0215(19) 0.0185(18) 0.0030(17)
O3 0.047(2) 0.042(2) 0.051(2) 0.021(2) 0.018(2) 0.0254(19)
N1 0.031(2) 0.030(2) 0.031(2) 0.013(2) 0.0119(19) 0.0062(19)
N2 0.031(2) 0.031(2) 0.033(2) 0.014(2) 0.008(2) 0.0021(19)
C1 0.028(3) 0.046(3) 0.032(3) 0.024(3) 0.015(2) 0.010(2)
C2 0.033(3) 0.047(3) 0.033(3) 0.025(3) 0.017(2) 0.013(3)
C3 0.050(4) 0.067(4) 0.050(4) 0.037(4) 0.020(3) 0.027(3)
C4 0.055(4) 0.091(6) 0.038(4) 0.039(4) 0.013(3) 0.030(4)
C5 0.048(4) 0.064(4) 0.026(3) 0.014(3) 0.007(3) 0.010(3)
C6 0.035(3) 0.044(3) 0.035(3) 0.017(3) 0.017(3) 0.008(3)
C7 0.042(3) 0.040(3) 0.045(3) 0.026(3) 0.020(3) 0.014(3)
C8 0.078(5) 0.052(4) 0.078(5) 0.042(4) 0.032(4) 0.025(4)
C9 0.048(4) 0.053(4) 0.038(3) 0.014(3) 0.018(3) 0.014(3)
C10 0.046(3) 0.048(4) 0.032(3) 0.012(3) 0.018(3) 0.012(3)
C11 0.073(5) 0.050(4) 0.057(4) 0.008(4) 0.024(4) 0.009(4)
C12 0.052(4) 0.076(5) 0.089(6) 0.044(5) 0.035(4) 0.025(4)
C13 0.035(3) 0.035(3) 0.042(3) 0.020(3) 0.021(3) 0.008(2)
C14 0.035(3) 0.049(4) 0.049(4) 0.027(3) 0.019(3) 0.006(3)
C15 0.033(3) 0.081(5) 0.057(4) 0.034(4) 0.016(3) 0.004(3)
C16 0.048(4) 0.097(6) 0.073(5) 0.038(5) 0.039(4) 0.009(4)
C17 0.063(5) 0.073(5) 0.064(5) 0.032(4) 0.042(4) 0.006(4)
C18 0.046(4) 0.049(4) 0.049(4) 0.020(3) 0.023(3) 0.004(3)
C19 0.030(3) 0.056(4) 0.044(3) 0.019(3) 0.013(3) 0.000(3)
C20 0.075(5) 0.057(5) 0.068(5) 0.018(4) 0.023(4) 0.012(4)
C21 0.048(4) 0.066(5) 0.052(4) 0.029(4) 0.013(3) 0.000(3)
C22 0.051(4) 0.074(5) 0.036(3) 0.017(3) 0.019(3) -0.007(4)
C23 0.080(6) 0.099(7) 0.089(7) 0.050(6) -0.008(5) -0.001(5)
C24 0.085(6) 0.108(7) 0.051(5) 0.007(5) 0.030(4) -0.008(5)
C25 0.035(3) 0.053(4) 0.035(3) 0.022(3) 0.018(3) 0.011(3)
C26 0.064(4) 0.058(4) 0.034(3) 0.011(3) 0.021(3) 0.014(3)
C27 0.082(6) 0.112(7) 0.032(4) 0.021(4) 0.025(4) 0.029(5)
C28 0.073(5) 0.153(9) 0.070(6) 0.080(6) 0.041(5) 0.048(6)
C29 0.067(5) 0.097(6) 0.081(6) 0.067(5) 0.042(4) 0.029(4)
C30 0.051(4) 0.060(4) 0.052(4) 0.033(4) 0.027(3) 0.011(3)
C31 0.040(3) 0.037(3) 0.033(3) 0.005(3) 0.013(3) 0.008(3)
C32 0.056(4) 0.043(4) 0.060(4) 0.025(3) 0.022(3) 0.017(3)
C33 0.080(5) 0.056(5) 0.075(5) 0.030(4) 0.021(4) 0.036(4)
C34 0.092(6) 0.073(6) 0.081(6) 0.016(5) 0.032(5) 0.058(5)
C35 0.091(6) 0.104(7) 0.090(6) 0.036(6) 0.058(5) 0.059(6)
C36 0.062(4) 0.068(5) 0.059(4) 0.021(4) 0.034(4) 0.032(4)
C37 0.039(3) 0.035(3) 0.052(4) 0.028(3) 0.014(3) 0.005(3)
C38 0.057(4) 0.039(4) 0.041(4) 0.016(3) 0.010(3) 0.007(3)
C39 0.091(6) 0.035(4) 0.048(4) 0.009(3) 0.006(4) -0.006(4)
C40 0.070(5) 0.052(5) 0.082(6) 0.034(5) -0.013(5) -0.022(4)
C41 0.047(4) 0.068(5) 0.129(8) 0.062(6) 0.024(5) 0.000(4)
C42 0.047(4) 0.048(4) 0.092(5) 0.034(4) 0.027(4) -0.001(3)
C43 0.034(3) 0.041(3) 0.036(3) 0.021(3) 0.021(2) 0.015(2)
C44 0.089(5) 0.048(4) 0.043(4) 0.025(3) 0.037(4) 0.025(4)
C45 0.120(7) 0.079(6) 0.048(4) 0.043(4) 0.040(5) 0.041(5)
C46 0.083(5) 0.111(7) 0.045(4) 0.048(5) 0.028(4) 0.043(5)
C47 0.049(4) 0.073(5) 0.049(4) 0.027(4) 0.018(3) 0.005(4)
C48 0.043(3) 0.053(4) 0.046(4) 0.025(3) 0.016(3) 0.004(3)
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 N2 1.740(4) . ?
Mo1 N1 1.745(4) . ?
Mo1 O3 1.883(4) . ?
Mo1 O1 1.884(4) . ?
Si1 O2 1.617(4) . ?
Si1 O1 1.627(4) . ?
Si1 C25 1.869(3) . ?
Si1 C31 1.877(3) . ?
Si2 O3 1.612(4) 2_765 ?
Si2 O2 1.614(4) . ?
Si2 C43 1.868(3) . ?
Si2 C37 1.884(4) . ?
O3 Si2 1.612(4) 2_765 ?
N1 C1 1.397(6) . ?
N2 C13 1.405(6) . ?
C1 C6 1.412(8) . ?
C1 C2 1.413(7) . ?
C2 C3 1.394(8) . ?
C2 C7 1.527(8) . ?
C3 C4 1.389(9) . ?
C3 H3 0.93 . ?
C4 C5 1.357(9) . ?
C4 H4 0.93 . ?
C5 C6 1.402(8) . ?
C5 H5 0.93 . ?
C6 C10 1.512(8) . ?
C7 C8 1.533(8) . ?
C7 C9 1.533(8) . ?
C7 H7 0.98 . ?
C8 H8A 0.96 . ?
C8 H8B 0.96 . ?
C8 H8C 0.96 . ?
C9 H9A 0.96 . ?
C9 H9B 0.96 . ?
C9 H9C 0.96 . ?
C10 C12 1.521(8) . ?
C10 C11 1.538(9) . ?
C10 H10 0.98 . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 H12A 0.96 . ?
C12 H12B 0.96 . ?
C12 H12C 0.96 . ?
C13 C14 1.406(8) . ?
C13 C18 1.411(8) . ?
C14 C15 1.390(8) . ?
C14 C19 1.516(8) . ?
C15 C16 1.385(9) . ?
C15 H15 0.93 . ?
C16 C17 1.379(10) . ?
C16 H16 0.93 . ?
C17 C18 1.392(8) . ?
C17 H17 0.93 . ?
C18 C22 1.520(8) . ?
C19 C21 1.512(8) . ?
C19 C20 1.528(9) . ?
C19 H19 0.98 . ?
C20 H20A 0.96 . ?
C20 H20B 0.96 . ?
C20 H20C 0.96 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 C23 1.489(11) . ?
C22 C24 1.531(10) . ?
C22 H22 0.98 . ?
C23 H23A 0.96 . ?
C23 H23B 0.96 . ?
C23 H23C 0.96 . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
C25 C26 1.39 . ?
C25 C30 1.39 . ?
C26 C27 1.39 . ?
C26 H26 0.93 . ?
C27 C28 1.39 . ?
C27 H27 0.93 . ?
C28 C29 1.39 . ?
C28 H28 0.93 . ?
C29 C30 1.39 . ?
C29 H29 0.93 . ?
C30 H30 0.93 . ?
C31 C32 1.39 . ?
C31 C36 1.39 . ?
C32 C33 1.39 . ?
C32 H32 0.93 . ?
C33 C34 1.39 . ?
C33 H33 0.93 . ?
C34 C35 1.39 . ?
C34 H34 0.93 . ?
C35 C36 1.39 . ?
C35 H35 0.93 . ?
C36 H36 0.93 . ?
C37 C38 1.39 . ?
C37 C42 1.39 . ?
C38 C39 1.39 . ?
C38 H38 0.93 . ?
C39 C40 1.39 . ?
C39 H39 0.93 . ?
C40 C41 1.39 . ?
C40 H40 0.93 . ?
C41 C42 1.39 . ?
C41 H41 0.93 . ?
C42 H42 0.93 . ?
C43 C44 1.39 . ?
C43 C48 1.39 . ?
C44 C45 1.39 . ?
C44 H44 0.93 . ?
C45 C46 1.39 . ?
C45 H45 0.93 . ?
C46 C47 1.39 . ?
C46 H46 0.93 . ?
C47 C48 1.39 . ?
C47 H47 0.93 . ?
C48 H48 0.93 . ?
C49 C51 1.48(2) 2_675 ?
C49 C50 1.68(2) . ?
C49 H49 0.93 . ?
C50 C51 1.31(2) . ?
C50 H50 0.93 . ?
C51 C49 1.48(2) 2_675 ?
C51 H51 0.93 . ?
 
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
N2 Mo1 N1 110.15(19) . . ?
N2 Mo1 O3 109.1(2) . . ?
N1 Mo1 O3 108.37(19) . . ?
N2 Mo1 O1 108.61(19) . . ?
N1 Mo1 O1 108.77(19) . . ?
O3 Mo1 O1 111.84(17) . . ?
O2 Si1 O1 108.8(2) . . ?
O2 Si1 C25 108.00(19) . . ?
O1 Si1 C25 109.1(2) . . ?
O2 Si1 C31 108.0(2) . . ?
O1 Si1 C31 111.5(2) . . ?
C25 Si1 C31 111.30(19) . . ?
O3 Si2 O2 110.3(2) 2_765 . ?
O3 Si2 C43 107.7(2) 2_765 . ?
O2 Si2 C43 108.01(19) . . ?
O3 Si2 C37 110.3(2) 2_765 . ?
O2 Si2 C37 105.9(2) . . ?
C43 Si2 C37 114.66(19) . . ?
Si1 O1 Mo1 174.9(3) . . ?
Si2 O2 Si1 161.7(3) . . ?
Si2 O3 Mo1 174.7(3) 2_765 . ?
C1 N1 Mo1 161.1(4) . . ?
C13 N2 Mo1 167.8(4) . . ?
N1 C1 C6 119.2(5) . . ?
N1 C1 C2 118.3(5) . . ?
C6 C1 C2 122.4(5) . . ?
C3 C2 C1 117.6(5) . . ?
C3 C2 C7 121.7(5) . . ?
C1 C2 C7 120.7(4) . . ?
C4 C3 C2 120.0(6) . . ?
C4 C3 H3 120 . . ?
C2 C3 H3 120 . . ?
C5 C4 C3 121.9(6) . . ?
C5 C4 H4 119 . . ?
C3 C4 H4 119 . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 116.8(5) . . ?
C5 C6 C10 122.1(5) . . ?
C1 C6 C10 121.0(5) . . ?
C2 C7 C8 113.0(5) . . ?
C2 C7 C9 110.6(5) . . ?
C8 C7 C9 110.3(5) . . ?
C2 C7 H7 107.6 . . ?
C8 C7 H7 107.6 . . ?
C9 C7 H7 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 C12 109.1(5) . . ?
C6 C10 C11 114.5(5) . . ?
C12 C10 C11 110.9(5) . . ?
C6 C10 H10 107.4 . . ?
C12 C10 H10 107.3 . . ?
C11 C10 H10 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 121.2(5) . . ?
C14 C13 C18 121.5(5) . . ?
N2 C13 C18 117.4(5) . . ?
C15 C14 C13 117.9(6) . . ?
C15 C14 C19 119.5(5) . . ?
C13 C14 C19 122.6(5) . . ?
C16 C15 C14 121.5(6) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C17 C16 C15 119.9(6) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 121.3(6) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C13 117.9(6) . . ?
C17 C18 C22 121.4(6) . . ?
C13 C18 C22 120.7(5) . . ?
C21 C19 C14 112.0(5) . . ?
C21 C19 C20 111.1(5) . . ?
C14 C19 C20 110.8(5) . . ?
C21 C19 H19 107.6 . . ?
C14 C19 H19 107.6 . . ?
C20 C19 H19 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C18 110.3(6) . . ?
C23 C22 C24 111.5(7) . . ?
C18 C22 C24 114.2(6) . . ?
C23 C22 H22 106.8 . . ?
C18 C22 H22 106.8 . . ?
C24 C22 H22 106.8 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 120 . . ?
C26 C25 Si1 119.5(2) . . ?
C30 C25 Si1 120.1(2) . . ?
C27 C26 C25 120 . . ?
C27 C26 H26 120 . . ?
C25 C26 H26 120 . . ?
C26 C27 C28 120 . . ?
C26 C27 H27 120 . . ?
C28 C27 H27 120 . . ?
C29 C28 C27 120 . . ?
C29 C28 H28 120 . . ?
C27 C28 H28 120 . . ?
C30 C29 C28 120 . . ?
C30 C29 H29 120 . . ?
C28 C29 H29 120 . . ?
C29 C30 C25 120 . . ?
C29 C30 H30 120 . . ?
C25 C30 H30 120 . . ?
C32 C31 C36 120 . . ?
C32 C31 Si1 121.1(2) . . ?
C36 C31 Si1 118.9(2) . . ?
C31 C32 C33 120 . . ?
C31 C32 H32 120 . . ?
C33 C32 H32 120 . . ?
C34 C33 C32 120 . . ?
C34 C33 H33 120 . . ?
C32 C33 H33 120 . . ?
C33 C34 C35 120 . . ?
C33 C34 H34 120 . . ?
C35 C34 H34 120 . . ?
C34 C35 C36 120 . . ?
C34 C35 H35 120 . . ?
C36 C35 H35 120 . . ?
C35 C36 C31 120 . . ?
C35 C36 H36 120 . . ?
C31 C36 H36 120 . . ?
C38 C37 C42 120 . . ?
C38 C37 Si2 119.8(2) . . ?
C42 C37 Si2 120.2(2) . . ?
C37 C38 C39 120 . . ?
C37 C38 H38 120 . . ?
C39 C38 H38 120 . . ?
C38 C39 C40 120 . . ?
C38 C39 H39 120 . . ?
C40 C39 H39 120 . . ?
C41 C40 C39 120 . . ?
C41 C40 H40 120 . . ?
C39 C40 H40 120 . . ?
C42 C41 C40 120 . . ?
C42 C41 H41 120 . . ?
C40 C41 H41 120 . . ?
C41 C42 C37 120 . . ?
C41 C42 H42 120 . . ?
C37 C42 H42 120 . . ?
C44 C43 C48 120 . . ?
C44 C43 Si2 121.8(2) . . ?
C48 C43 Si2 118.1(2) . . ?
C43 C44 C45 120 . . ?
C43 C44 H44 120 . . ?
C45 C44 H44 120 . . ?
C44 C45 C46 120 . . ?
C44 C45 H45 120 . . ?
C46 C45 H45 120 . . ?
C47 C46 C45 120 . . ?
C47 C46 H46 120 . . ?
C45 C46 H46 120 . . ?
C46 C47 C48 120 . . ?
C46 C47 H47 120 . . ?
C48 C47 H47 120 . . ?
C47 C48 C43 120 . . ?
C47 C48 H48 120 . . ?
C43 C48 H48 120 . . ?
C51 C49 C50 142.8(17) 2_675 . ?
C51 C49 H49 108.5 2_675 . ?
C50 C49 H49 108.7 . . ?
C51 C50 C49 81.2(16) . . ?
C51 C50 H50 139.6 . . ?
C49 C50 H50 139.1 . . ?
C50 C51 C49 136(2) . 2_675 ?
C50 C51 H51 111.9 . . ?
C49 C51 H51 112.4 2_675 . ?
 
 
 
data_lkmo2
 
_audit_creation_date            1999-08-27T15:56:50-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C64 H76 Mo1 N4 O6 Si4'
_chemical_formula_structural            'C64 H76 N4 O6 SI4 MO'
_chemical_formula_sum                   'C64 H76 Mo2 N4 O6 Si4'
_chemical_formula_weight                1301.53
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/c'
_symmetry_space_group_name_Hall         '-P 2ybc'
_symmetry_Int_Tables_number             14
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
 
_cell_length_a                          12.395(2)
_cell_length_b                          15.831(3)
_cell_length_c                          17.246(3)
_cell_angle_alpha                       90
_cell_angle_beta                        100.07(3)
_cell_angle_gamma                       90
_cell_volume                            3332.0(10)
_cell_formula_units_Z                   2
_cell_measurement_temperature           293(2)
_cell_measurement_reflns_used           25
_cell_measurement_theta_min             0
_cell_measurement_theta_max             0
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   Orange
_exptl_crystal_size_max                 0.4
_exptl_crystal_size_mid                 0.3
_exptl_crystal_size_min                 0.2
_exptl_crystal_density_diffrn           1.297
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1352
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.498
_exptl_absorpt_factor_muR               0
_exptl_absorpt_correction_type          psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_absorpt_correction_T_min         0.2933
_exptl_absorpt_correction_T_max         0.9981
_exptl_absorpt_correction_T_ave         0.5609
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_measurement_device              'Enraf Nonius CAD4'
_diffrn_measurement_method              'non-profiled omega/2theta scans'
_diffrn_standards_number                2
_diffrn_standards_interval_time         60
_diffrn_standards_decay_%               1
_diffrn_standards_decay_corr_max        1.03
_diffrn_standards_decay_corr_min        0.973
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
3 -6 3
5 3 -3
 
_diffrn_reflns_number                   5846
_diffrn_reflns_av_R_equivalents         0
_diffrn_reflns_av_sigmaI/netI           0.1991
_diffrn_reflns_limit_h_min              -14
_diffrn_reflns_limit_h_max              14
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              18
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              20
_diffrn_reflns_theta_min                1.67
_diffrn_reflns_theta_max                25
_diffrn_reflns_theta_full               25
_diffrn_measured_fraction_theta_full
                                        0.998
_diffrn_measured_fraction_theta_max
                                        0.998
_reflns_number_total                    5846
_reflns_number_gt                       2470
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'CAD4/PC (Enraf Nonius, 1992)'
_computing_cell_refinement              'CAD4/PC (Enraf Nonius, 1992)'
_computing_data_reduction               'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution           SHELXS-97(Sheldrick,1997)
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1998)'
 
#----------------------------------------------------------------------------#
#                   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^ > 2sigma(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
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            SHELXL
_refine_ls_extinction_expression
                                    Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef              0.0018(5)
_refine_ls_number_reflns                5846
_refine_ls_number_parameters            319
_refine_ls_number_restraints            106
_refine_ls_R_factor_all                 0.2106
_refine_ls_R_factor_gt                  0.0867
_refine_ls_wR_factor_ref                0.2454
_refine_ls_wR_factor_gt                 0.2059
_refine_ls_goodness_of_fit_ref          0.923
_refine_ls_restrained_S_all             0.919
_refine_ls_shift/su_max                 0.002
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.951
_refine_diff_density_min                -1.013
_refine_diff_density_rms                0.126
 
#----------------------------------------------------------------------------#
#                   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'
Si Si 0.0817 0.0704 '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 0.51564(7) 0.35343(6) 0.51738(6) 0.0514(3) Uani 1 1 d U . .
Si1 Si 0.2729(2) 0.36744(18) 0.39867(16) 0.0468(7) Uani 1 1 d U . .
Si2 Si 0.7492(2) 0.45983(18) 0.52762(16) 0.0459(7) Uani 1 1 d U . .
O1 O 0.6209(4) 0.4394(4) 0.5257(4) 0.0536(17) Uani 1 1 d U . .
O2 O 0.4038(4) 0.3517(4) 0.4268(4) 0.0540(16) Uani 1 1 d U . .
O3 O 0.7750(5) 0.5598(4) 0.5522(4) 0.0470(16) Uani 1 1 d U . .
N1 N 0.4580(7) 0.3567(6) 0.5999(5) 0.068(2) Uani 1 1 d U . .
N2 N 0.5846(6) 0.2613(6) 0.5136(6) 0.068(3) Uani 1 1 d U A .
C1 C 0.1954(5) 0.2681(4) 0.4120(5) 0.051(2) Uani 1 1 d GU . .
C2 C 0.0965(6) 0.2699(4) 0.4395(5) 0.074(3) Uani 1 1 d GU . .
H2 H 0.0684 0.3209 0.4537 0.14(2) Uiso 1 1 calc R . .
C3 C 0.0395(5) 0.1953(6) 0.4457(5) 0.093(4) Uani 1 1 d GU . .
H3 H -0.0267 0.1964 0.4641 0.14(2) Uiso 1 1 calc R . .
C4 C 0.0814(8) 0.1189(4) 0.4244(6) 0.100(4) Uani 1 1 d GU . .
H4 H 0.0433 0.069 0.4286 0.14(2) Uiso 1 1 calc R . .
C5 C 0.1803(8) 0.1172(4) 0.3970(6) 0.108(5) Uani 1 1 d GU . .
H5 H 0.2084 0.0661 0.3827 0.14(2) Uiso 1 1 calc R . .
C6 C 0.2373(5) 0.1918(5) 0.3907(5) 0.091(4) Uani 1 1 d GU . .
H6 H 0.3035 0.1907 0.3724 0.14(2) Uiso 1 1 calc R . .
C7 C 0.2546(5) 0.3967(5) 0.2925(3) 0.051(2) Uani 1 1 d GU . .
C8 C 0.1507(5) 0.3933(5) 0.2466(5) 0.074(3) Uani 1 1 d GU . .
H8 H 0.0916 0.374 0.2683 0.15(3) Uiso 1 1 calc R . .
C9 C 0.1351(6) 0.4185(6) 0.1683(4) 0.103(5) Uani 1 1 d GU . .
H9 H 0.0655 0.4163 0.1376 0.15(3) Uiso 1 1 calc R . .
C10 C 0.2234(8) 0.4472(6) 0.1358(3) 0.107(5) Uani 1 1 d GU . .
H10 H 0.2129 0.4642 0.0834 0.15(3) Uiso 1 1 calc R . .
C11 C 0.3273(7) 0.4507(6) 0.1817(5) 0.095(4) Uani 1 1 d GU . .
H11 H 0.3864 0.4699 0.16 0.15(3) Uiso 1 1 calc R . .
C12 C 0.3429(4) 0.4254(5) 0.2601(4) 0.066(3) Uani 1 1 d GU . .
H12 H 0.4125 0.4277 0.2908 0.15(3) Uiso 1 1 calc R . .
C13 C 0.7903(5) 0.4434(4) 0.4298(3) 0.055(2) Uani 1 1 d GU . .
C14 C 0.7398(6) 0.3804(4) 0.3803(4) 0.069(3) Uani 1 1 d GU . .
H14 H 0.6846 0.3478 0.3955 0.12(2) Uiso 1 1 calc R . .
C15 C 0.7716(6) 0.3661(5) 0.3080(4) 0.090(4) Uani 1 1 d GU . .
H15 H 0.7377 0.324 0.2748 0.12(2) Uiso 1 1 calc R . .
C16 C 0.8540(6) 0.4149(6) 0.2853(4) 0.082(4) Uani 1 1 d GU . .
H16 H 0.8752 0.4054 0.2369 0.12(2) Uiso 1 1 calc R . .
C17 C 0.9045(5) 0.4779(5) 0.3349(4) 0.080(4) Uani 1 1 d GU . .
H17 H 0.9597 0.5106 0.3197 0.12(2) Uiso 1 1 calc R . .
C18 C 0.8727(5) 0.4922(4) 0.4071(4) 0.062(3) Uani 1 1 d GU . .
H18 H 0.9066 0.5344 0.4403 0.12(2) Uiso 1 1 calc R . .
C19 C 0.8308(5) 0.3900(4) 0.6044(4) 0.048(2) Uani 1 1 d GU . .
C20 C 0.9210(5) 0.3454(5) 0.5885(4) 0.066(3) Uani 1 1 d GU . .
H20 H 0.9386 0.3467 0.5382 0.12(2) Uiso 1 1 calc R . .
C21 C 0.9851(5) 0.2988(5) 0.6477(5) 0.083(4) Uani 1 1 d GU . .
H21 H 1.0454 0.269 0.637 0.12(2) Uiso 1 1 calc R . .
C22 C 0.9588(6) 0.2968(5) 0.7228(4) 0.094(4) Uani 1 1 d GU . .
H22 H 1.0017 0.2657 0.7624 0.12(2) Uiso 1 1 calc R . .
C23 C 0.8686(7) 0.3414(5) 0.7387(3) 0.088(4) Uani 1 1 d GU . .
H23 H 0.8511 0.3401 0.789 0.12(2) Uiso 1 1 calc R . .
C24 C 0.8046(5) 0.3880(4) 0.6795(4) 0.066(3) Uani 1 1 d GU . .
H24 H 0.7442 0.4178 0.6902 0.12(2) Uiso 1 1 calc R . .
C25 C 0.4155(9) 0.3340(8) 0.6718(7) 0.069(3) Uani 1 1 d U . .
C26 C 0.4095(12) 0.4151(9) 0.7189(8) 0.103(4) Uani 1 1 d U . .
H26A H 0.3623 0.4549 0.6875 0.10(2) Uiso 1 1 calc R . .
H26B H 0.4816 0.4388 0.7329 0.10(2) Uiso 1 1 calc R . .
H26C H 0.3809 0.4026 0.7659 0.10(2) Uiso 1 1 calc R . .
C27 C 0.4970(10) 0.2735(10) 0.7242(9) 0.111(5) Uani 1 1 d U . .
H27A H 0.5687 0.2984 0.7339 0.16(4) Uiso 1 1 calc R . .
H27B H 0.4998 0.2205 0.6976 0.16(4) Uiso 1 1 calc R . .
H27C H 0.4727 0.2642 0.7734 0.16(4) Uiso 1 1 calc R . .
C28 C 0.3038(10) 0.2962(10) 0.6507(8) 0.100(5) Uani 1 1 d U . .
H28A H 0.2775 0.2806 0.6978 0.09(2) Uiso 1 1 calc R . .
H28B H 0.3072 0.247 0.6187 0.09(2) Uiso 1 1 calc R . .
H28C H 0.2548 0.3368 0.6219 0.09(2) Uiso 1 1 calc R . .
C29 C 0.6256(9) 0.1720(7) 0.5222(8) 0.073(3) Uani 1 1 d DU . .
C30A C 0.6969(19) 0.1624(17) 0.5969(13) 0.108(7) Uiso 0.615(11) 1 d PDU A 1
H30A H 0.7503 0.2069 0.6036 0.163 Uiso 0.615(11) 1 calc PR A 1
H30B H 0.7335 0.1088 0.5986 0.163 Uiso 0.615(11) 1 calc PR A 1
H30C H 0.6546 0.1651 0.6384 0.163 Uiso 0.615(11) 1 calc PR A 1
C31A C 0.5324(18) 0.1079(17) 0.5033(16) 0.114(7) Uiso 0.615(11) 1 d PDU A 1
H31A H 0.4894 0.1207 0.4527 0.17 Uiso 0.615(11) 1 calc PR A 1
H31B H 0.4868 0.1108 0.5429 0.17 Uiso 0.615(11) 1 calc PR A 1
H31C H 0.5624 0.0521 0.5023 0.17 Uiso 0.615(11) 1 calc PR A 1
C32A C 0.701(2) 0.1620(18) 0.4573(16) 0.129(8) Uiso 0.615(11) 1 d PDU A 1
H32A H 0.6567 0.1659 0.4059 0.193 Uiso 0.615(11) 1 calc PR A 1
H32B H 0.7367 0.108 0.4631 0.193 Uiso 0.615(11) 1 calc PR A 1
H32C H 0.7552 0.2059 0.4637 0.193 Uiso 0.615(11) 1 calc PR A 1
C30B C 0.749(2) 0.174(3) 0.544(2) 0.108(7) Uiso 0.385(11) 1 d PDU A 2
H30D H 0.7699 0.1984 0.5956 0.163 Uiso 0.385(11) 1 calc PR A 2
H30E H 0.7793 0.2064 0.5064 0.163 Uiso 0.385(11) 1 calc PR A 2
H30F H 0.7771 0.1169 0.545 0.163 Uiso 0.385(11) 1 calc PR A 2
C31B C 0.560(3) 0.120(2) 0.5780(18) 0.114(7) Uiso 0.385(11) 1 d PDU A 2
H31D H 0.4824 0.1242 0.5585 0.17 Uiso 0.385(11) 1 calc PR A 2
H31E H 0.5758 0.1419 0.6305 0.17 Uiso 0.385(11) 1 calc PR A 2
H31F H 0.5811 0.0613 0.5784 0.17 Uiso 0.385(11) 1 calc PR A 2
C32B C 0.599(3) 0.129(3) 0.447(3) 0.129(8) Uiso 0.385(11) 1 d PDU A 2
H32D H 0.5209 0.1255 0.4317 0.193 Uiso 0.385(11) 1 calc PR A 2
H32E H 0.6296 0.0732 0.4515 0.193 Uiso 0.385(11) 1 calc PR A 2
H32F H 0.629 0.1601 0.4078 0.193 Uiso 0.385(11) 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
Mo1 0.0407(4) 0.0500(6) 0.0586(6) -0.0003(5) -0.0052(4) -0.0035(5)
Si1 0.0419(13) 0.0475(19) 0.0462(16) -0.0047(13) -0.0055(12) -0.0016(11)
Si2 0.0408(13) 0.0405(17) 0.0511(17) -0.0048(13) -0.0071(12) -0.0026(11)
O1 0.029(3) 0.076(5) 0.051(4) 0.005(4) -0.008(3) -0.010(3)
O2 0.032(3) 0.052(4) 0.069(4) -0.003(4) -0.012(3) 0.000(3)
O3 0.046(3) 0.036(4) 0.058(4) 0.001(3) 0.005(3) 0.001(3)
N1 0.065(5) 0.067(7) 0.072(5) 0.001(5) 0.011(4) -0.008(5)
N2 0.047(5) 0.059(5) 0.088(7) -0.009(5) -0.013(4) 0.019(4)
C1 0.051(5) 0.056(6) 0.041(6) -0.011(4) -0.002(5) -0.010(4)
C2 0.078(7) 0.070(7) 0.079(8) -0.007(7) 0.029(7) -0.027(6)
C3 0.095(9) 0.073(8) 0.113(11) -0.004(9) 0.025(8) -0.043(7)
C4 0.119(10) 0.073(8) 0.100(11) 0.012(8) -0.004(8) -0.021(7)
C5 0.125(11) 0.055(7) 0.141(15) -0.013(9) 0.012(10) -0.015(7)
C6 0.094(9) 0.051(6) 0.130(13) -0.006(8) 0.019(8) 0.003(6)
C7 0.060(5) 0.042(6) 0.048(5) -0.009(4) 0.001(4) 0.003(4)
C8 0.075(6) 0.081(9) 0.058(6) -0.005(6) -0.016(5) -0.001(6)
C9 0.117(9) 0.092(12) 0.078(8) 0.021(8) -0.044(7) -0.017(9)
C10 0.161(12) 0.082(11) 0.064(8) 0.015(8) -0.017(7) -0.024(10)
C11 0.123(9) 0.103(12) 0.060(7) 0.004(7) 0.022(7) -0.015(9)
C12 0.080(6) 0.059(8) 0.058(6) 0.001(6) 0.010(5) -0.009(6)
C13 0.053(5) 0.048(7) 0.061(5) -0.012(4) 0.002(4) -0.005(4)
C14 0.092(8) 0.052(8) 0.063(7) -0.016(5) 0.018(6) -0.027(6)
C15 0.087(8) 0.114(12) 0.067(7) -0.031(8) 0.011(7) -0.029(7)
C16 0.069(7) 0.114(12) 0.063(8) -0.015(7) 0.010(6) -0.011(6)
C17 0.075(8) 0.089(11) 0.080(9) -0.020(7) 0.021(7) -0.017(6)
C18 0.058(6) 0.057(8) 0.070(7) -0.002(5) 0.012(6) -0.011(5)
C19 0.045(5) 0.031(5) 0.062(5) -0.009(4) -0.006(4) 0.000(4)
C20 0.050(5) 0.061(8) 0.085(7) 0.004(6) 0.001(5) 0.003(5)
C21 0.067(7) 0.057(9) 0.116(9) 0.018(8) -0.005(7) 0.016(6)
C22 0.085(9) 0.088(11) 0.093(8) 0.009(8) -0.028(7) 0.014(7)
C23 0.098(9) 0.079(11) 0.077(8) 0.019(7) -0.010(6) 0.011(7)
C24 0.081(7) 0.049(7) 0.064(6) 0.010(5) 0.002(6) 0.001(5)
C25 0.065(6) 0.072(9) 0.066(7) 0.011(5) 0.002(5) 0.000(5)
C26 0.151(13) 0.083(9) 0.076(9) -0.009(7) 0.025(9) -0.019(8)
C27 0.086(8) 0.126(13) 0.120(12) 0.054(10) 0.020(8) 0.028(9)
C28 0.079(7) 0.123(13) 0.097(11) -0.001(9) 0.010(7) -0.033(8)
C29 0.067(7) 0.053(6) 0.088(9) -0.013(6) -0.020(7) 0.001(5)
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 N2 1.698(9) . ?
Mo1 N1 1.701(8) . ?
Mo1 O1 1.873(6) . ?
Mo1 O2 1.899(6) . ?
Si1 O3 1.605(7) 3_666 ?
Si1 O2 1.630(6) . ?
Si1 C7 1.863(6) . ?
Si1 C1 1.877(6) . ?
Si2 O1 1.618(6) . ?
Si2 O3 1.654(7) . ?
Si2 C13 1.863(6) . ?
Si2 C19 1.879(6) . ?
O3 Si1 1.605(7) 3_666 ?
N1 C25 1.474(13) . ?
N2 C29 1.500(13) . ?
C1 C2 1.39 . ?
C1 C6 1.39 . ?
C2 C3 1.39 . ?
C2 H2 0.93 . ?
C3 C4 1.39 . ?
C3 H3 0.93 . ?
C4 C5 1.39 . ?
C4 H4 0.93 . ?
C5 C6 1.39 . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
C7 C8 1.39 . ?
C7 C12 1.39 . ?
C8 C9 1.39 . ?
C8 H8 0.93 . ?
C9 C10 1.39 . ?
C9 H9 0.93 . ?
C10 C11 1.39 . ?
C10 H10 0.93 . ?
C11 C12 1.39 . ?
C11 H11 0.93 . ?
C12 H12 0.93 . ?
C13 C14 1.39 . ?
C13 C18 1.39 . ?
C14 C15 1.39 . ?
C14 H14 0.93 . ?
C15 C16 1.39 . ?
C15 H15 0.93 . ?
C16 C17 1.39 . ?
C16 H16 0.93 . ?
C17 C18 1.39 . ?
C17 H17 0.93 . ?
C18 H18 0.93 . ?
C19 C20 1.39 . ?
C19 C24 1.39 . ?
C20 C21 1.39 . ?
C20 H20 0.93 . ?
C21 C22 1.39 . ?
C21 H21 0.93 . ?
C22 C23 1.39 . ?
C22 H22 0.93 . ?
C23 C24 1.39 . ?
C23 H23 0.93 . ?
C24 H24 0.93 . ?
C25 C28 1.494(15) . ?
C25 C26 1.528(17) . ?
C25 C27 1.562(16) . ?
C26 H26A 0.96 . ?
C26 H26B 0.96 . ?
C26 H26C 0.96 . ?
C27 H27A 0.96 . ?
C27 H27B 0.96 . ?
C27 H27C 0.96 . ?
C28 H28A 0.96 . ?
C28 H28B 0.96 . ?
C28 H28C 0.96 . ?
C29 C30A 1.44(2) . ?
C29 C32B 1.45(4) . ?
C29 C30B 1.51(3) . ?
C29 C31A 1.53(2) . ?
C29 C32A 1.586(19) . ?
C29 C31B 1.60(3) . ?
C30A H30A 0.96 . ?
C30A H30B 0.96 . ?
C30A H30C 0.96 . ?
C31A H31A 0.96 . ?
C31A H31B 0.96 . ?
C31A H31C 0.96 . ?
C32A H32A 0.96 . ?
C32A H32B 0.96 . ?
C32A H32C 0.96 . ?
C30B H30D 0.96 . ?
C30B H30E 0.96 . ?
C30B H30F 0.96 . ?
C31B H31D 0.96 . ?
C31B H31E 0.96 . ?
C31B H31F 0.96 . ?
C32B H32D 0.96 . ?
C32B H32E 0.96 . ?
C32B H32F 0.96 . ?
 
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
N2 Mo1 N1 110.2(5) . . ?
N2 Mo1 O1 106.2(4) . . ?
N1 Mo1 O1 107.6(4) . . ?
N2 Mo1 O2 104.8(4) . . ?
N1 Mo1 O2 109.6(4) . . ?
O1 Mo1 O2 118.1(3) . . ?
O3 Si1 O2 113.2(4) 3_666 . ?
O3 Si1 C7 110.4(4) 3_666 . ?
O2 Si1 C7 105.9(3) . . ?
O3 Si1 C1 107.0(3) 3_666 . ?
O2 Si1 C1 109.9(4) . . ?
C7 Si1 C1 110.6(4) . . ?
O1 Si2 O3 110.0(4) . . ?
O1 Si2 C13 112.1(3) . . ?
O3 Si2 C13 107.1(3) . . ?
O1 Si2 C19 107.6(3) . . ?
O3 Si2 C19 109.1(3) . . ?
C13 Si2 C19 110.9(3) . . ?
Si2 O1 Mo1 144.6(4) . . ?
Si1 O2 Mo1 142.0(4) . . ?
Si1 O3 Si2 138.5(4) 3_666 . ?
C25 N1 Mo1 163.9(9) . . ?
C29 N2 Mo1 165.9(9) . . ?
C2 C1 C6 120 . . ?
C2 C1 Si1 121.8(4) . . ?
C6 C1 Si1 118.2(4) . . ?
C1 C2 C3 120 . . ?
C1 C2 H2 120 . . ?
C3 C2 H2 120 . . ?
C4 C3 C2 120 . . ?
C4 C3 H3 120 . . ?
C2 C3 H3 120 . . ?
C3 C4 C5 120 . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
C6 C5 C4 120 . . ?
C6 C5 H5 120 . . ?
C4 C5 H5 120 . . ?
C5 C6 C1 120 . . ?
C5 C6 H6 120 . . ?
C1 C6 H6 120 . . ?
C8 C7 C12 120 . . ?
C8 C7 Si1 119.4(4) . . ?
C12 C7 Si1 120.5(4) . . ?
C9 C8 C7 120 . . ?
C9 C8 H8 120 . . ?
C7 C8 H8 120 . . ?
C8 C9 C10 120 . . ?
C8 C9 H9 120 . . ?
C10 C9 H9 120 . . ?
C9 C10 C11 120 . . ?
C9 C10 H10 120 . . ?
C11 C10 H10 120 . . ?
C12 C11 C10 120 . . ?
C12 C11 H11 120 . . ?
C10 C11 H11 120 . . ?
C11 C12 C7 120 . . ?
C11 C12 H12 120 . . ?
C7 C12 H12 120 . . ?
C14 C13 C18 120 . . ?
C14 C13 Si2 119.4(4) . . ?
C18 C13 Si2 120.6(4) . . ?
C15 C14 C13 120 . . ?
C15 C14 H14 120 . . ?
C13 C14 H14 120 . . ?
C16 C15 C14 120 . . ?
C16 C15 H15 120 . . ?
C14 C15 H15 120 . . ?
C15 C16 C17 120 . . ?
C15 C16 H16 120 . . ?
C17 C16 H16 120 . . ?
C16 C17 C18 120 . . ?
C16 C17 H17 120 . . ?
C18 C17 H17 120 . . ?
C17 C18 C13 120 . . ?
C17 C18 H18 120 . . ?
C13 C18 H18 120 . . ?
C20 C19 C24 120 . . ?
C20 C19 Si2 120.8(4) . . ?
C24 C19 Si2 119.0(4) . . ?
C19 C20 C21 120 . . ?
C19 C20 H20 120 . . ?
C21 C20 H20 120 . . ?
C22 C21 C20 120 . . ?
C22 C21 H21 120 . . ?
C20 C21 H21 120 . . ?
C23 C22 C21 120 . . ?
C23 C22 H22 120 . . ?
C21 C22 H22 120 . . ?
C22 C23 C24 120 . . ?
C22 C23 H23 120 . . ?
C24 C23 H23 120 . . ?
C23 C24 C19 120 . . ?
C23 C24 H24 120 . . ?
C19 C24 H24 120 . . ?
N1 C25 C28 110.2(10) . . ?
N1 C25 C26 107.5(10) . . ?
C28 C25 C26 109.7(10) . . ?
N1 C25 C27 110.2(9) . . ?
C28 C25 C27 111.9(11) . . ?
C26 C25 C27 107.2(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30A C29 C32B 139(2) . . ?
C30A C29 N2 109.4(13) . . ?
C32B C29 N2 109(2) . . ?
C30A C29 C30B 48.6(11) . . ?
C32B C29 C30B 107(2) . . ?
N2 C29 C30B 108.7(17) . . ?
C30A C29 C31A 116.4(17) . . ?
C32B C29 C31A 56.9(15) . . ?
N2 C29 C31A 111.9(13) . . ?
C30B C29 C31A 139(2) . . ?
C30A C29 C32A 106.0(15) . . ?
C32B C29 C32A 52.5(12) . . ?
N2 C29 C32A 104.8(14) . . ?
C30B C29 C32A 58.9(16) . . ?
C31A C29 C32A 107.4(15) . . ?
C30A C29 C31B 72.8(17) . . ?
C32B C29 C31B 104(2) . . ?
N2 C29 C31B 110.3(17) . . ?
C30B C29 C31B 117(2) . . ?
C31A C29 C31B 48.5(11) . . ?
C32A C29 C31B 143.0(19) . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29 C31A H31A 109.5 . . ?
C29 C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C29 C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C29 C32A H32A 109.5 . . ?
C29 C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C29 C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C29 C31B H31D 109.5 . . ?
C29 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C29 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C29 C32B H32D 109.5 . . ?
C29 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C29 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
 
 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 1999-11-11 at 16:39:49
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1beta3
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : moar1 dreduc struct psi_scan difabs
 
 
data_moar1
 
_audit_creation_date            1999-11-11T16:39:49-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1beta3
_audit_conform_dict_location    ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_publ_requested_category        FM
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C40 H40 Cl2 Mo1 N4'
_chemical_formula_structural            'C40 H40 N4 CL2 MO'
_chemical_formula_sum                   'C37.50 H47.50 Cl2 Mo N4'
_chemical_formula_weight                721.14
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 2/n'
_symmetry_space_group_name_Hall         '-P 2yac'
_symmetry_Int_Tables_number             13
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                          9.689(6)
_cell_length_b                          37.658(8)
_cell_length_c                          10.246(4)
_cell_angle_alpha                       90
_cell_angle_beta                        95.62(5)
_cell_angle_gamma                       90
_cell_volume                            3721(3)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)
_cell_measurement_reflns_used           25
_cell_measurement_theta_min             0
_cell_measurement_theta_max             0
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   orange
_exptl_crystal_size_max                 0.4
_exptl_crystal_size_mid                 0.3
_exptl_crystal_size_min                 0.3
_exptl_crystal_density_diffrn           1.287
_exptl_crystal_density_method           none
_exptl_crystal_F_000                    1506
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.526
_exptl_absorpt_factor_muR               0.123
_exptl_absorpt_correction_type          psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   3
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_absorpt_correction_T_min         0.7066
_exptl_absorpt_correction_T_max         0.8831
_exptl_absorpt_correction_T_ave         0.7987
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_detector                        'scintillation LiI'
_diffrn_detector_dtime                  1.195
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_ub_11             0.82042E-1
_diffrn_orient_matrix_ub_12             0.3539E-2
_diffrn_orient_matrix_ub_13             -0.50579E-1
_diffrn_orient_matrix_ub_21             -0.35936E-1
_diffrn_orient_matrix_ub_22             0.23908E-1
_diffrn_orient_matrix_ub_23             -0.28847E-1
_diffrn_orient_matrix_ub_31             0.51919E-1
_diffrn_orient_matrix_ub_32             0.11132E-1
_diffrn_orient_matrix_ub_33             0.79488E-1
_diffrn_measurement_device              '\k-geometry diffractometer'
_diffrn_measurement_device_type         'Enraf Nonius CAD4'
_diffrn_measurement_method              'non-profiled omega/2theta scans'
_diffrn_standards_number                2
_diffrn_standards_interval_time         60
_diffrn_standards_decay_%               7
_diffrn_standards_decay_corr_max        1.368
_diffrn_standards_decay_corr_min        0.95
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
-4 -16 1
-4 4 3
 
_diffrn_reflns_number                   6378
_diffrn_reflns_av_R_equivalents         0
_diffrn_reflns_av_sigmaI/netI           0.0851
_diffrn_reflns_limit_h_min              -11
_diffrn_reflns_limit_h_max              11
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              44
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              12
_diffrn_reflns_theta_min                2.07
_diffrn_reflns_theta_max                25.01
_reflns_number_total                    6378
_reflns_number_gt                       3822
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement              'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction               'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement         'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1998)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses 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 observed criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
_refine_ls_extinction_method            none
_refine_ls_number_reflns                6377
_refine_ls_number_parameters            385
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.1639
_refine_ls_R_factor_gt                  0.1067
_refine_ls_wR_factor_gt                 0.2893
_refine_ls_wR_factor_all                0.3358
_refine_ls_goodness_of_fit_gt           1.036
_refine_ls_goodness_of_fit_all          0.914
_refine_ls_restrained_S_all             0.917
_refine_ls_restrained_S_obs             1.036
_refine_ls_shift/su_max                 -0.106
_refine_ls_shift/su_mean                0.005
_refine_diff_density_max                2.245
_refine_diff_density_min                -3.886
_refine_diff_density_rms                0.248
 
#----------------------------------------------------------------------------#
#                   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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_group
Mo1 Mo 0.96714(9) 0.16618(3) 0.02503(8) 0.0321(3) Uani 1 d . .
Cl1 Cl 0.7237(3) 0.17835(9) 0.0136(3) 0.0447(8) Uani 1 d . .
Cl2 Cl 1.2111(3) 0.17787(8) 0.0344(3) 0.0419(7) Uani 1 d . .
N1 N 0.9573(9) 0.1347(3) -0.1043(8) 0.040(2) Uani 1 d . .
N2 N 0.9734(8) 0.1388(2) 0.1644(8) 0.033(2) Uani 1 d . .
C1 C 0.9461(7) 0.1018(2) -0.1623(7) 0.037(3) Uani 1 d G .
C2 C 0.8324(7) 0.0955(2) -0.2528(7) 0.042(3) Uani 1 d G .
C3 C 0.8099(7) 0.0617(2) -0.3054(7) 0.057(4) Uani 1 d G .
H3 H 0.7338(9) 0.0575(3) -0.3660(9) 0.07(3) Uiso 1 calc R .
C4 C 0.9011(9) 0.0343(2) -0.2674(8) 0.061(4) Uani 1 d G .
H4 H 0.8860(12) 0.0117(2) -0.3026(11) 0.07(3) Uiso 1 calc R .
C5 C 1.0148(8) 0.0406(2) -0.1769(8) 0.055(3) Uani 1 d G .
H5 H 1.0758(11) 0.0223(2) -0.1514(11) 0.07(3) Uiso 1 calc R .
C6 C 1.0374(6) 0.0744(2) -0.1243(7) 0.041(3) Uani 1 d G .
C7 C 0.7364(12) 0.1268(4) -0.2994(11) 0.045(3) Uani 1 d . .
H7 H 0.7650(12) 0.1475(4) -0.2451(11) 0.06(4) Uiso 1 calc R .
C8 C 0.5882(17) 0.1180(6) -0.276(3) 0.120(9) Uani 1 d . .
H8A H 0.583(3) 0.114(3) -0.184(3) 0.12(4) Uiso 1 calc R .
H8B H 0.559(5) 0.097(2) -0.324(10) 0.12(4) Uiso 1 calc R .
H8C H 0.529(3) 0.1375(16) -0.305(12) 0.12(4) Uiso 1 calc R .
C9 C 0.753(3) 0.1360(7) -0.4355(19) 0.133(10) Uani 1 d . .
H9A H 0.741(17) 0.1151(12) -0.489(3) 0.16(6) Uiso 1 calc R .
H9B H 0.844(7) 0.146(4) -0.441(3) 0.16(6) Uiso 1 calc R .
H9C H 0.685(12) 0.153(4) -0.466(6) 0.16(6) Uiso 1 calc R .
C10 C 0.9762(7) 0.1110(2) 0.2510(6) 0.042(3) Uani 1 d G .
C11 C 0.8797(7) 0.0836(2) 0.2354(7) 0.047(3) Uani 1 d G .
C12 C 0.8883(9) 0.0552(2) 0.3224(9) 0.071(4) Uani 1 d G .
H12 H 0.8237(12) 0.0369(3) 0.3120(12) 0.14(5) Uiso 1 calc R .
C13 C 0.9933(10) 0.0542(2) 0.4250(8) 0.072(5) Uani 1 d G .
H13 H 0.9990(14) 0.0352(3) 0.4832(11) 0.14(5) Uiso 1 calc R .
C14 C 1.0897(8) 0.0815(3) 0.4406(7) 0.064(4) Uani 1 d G .
H14 H 1.1600(10) 0.0808(4) 0.5092(9) 0.14(5) Uiso 1 calc R .
C15 C 1.0812(7) 0.1100(2) 0.3536(7) 0.049(3) Uani 1 d G .
C16 C 1.1674(12) 0.0818(4) -0.0320(12) 0.049(3) Uani 1 d . .
H16 H 1.1476(12) 0.1022(4) 0.0227(12) 0.03(3) Uiso 1 calc R .
C17 C 1.207(2) 0.0503(5) 0.0603(17) 0.092(6) Uani 1 d . .
H17A H 1.125(3) 0.042(2) 0.098(9) 0.11(4) Uiso 1 calc R .
H17B H 1.275(9) 0.0578(9) 0.129(7) 0.11(4) Uiso 1 calc R .
H17C H 1.244(12) 0.0314(13) 0.012(3) 0.11(4) Uiso 1 calc R .
C18 C 1.2838(15) 0.0927(5) -0.1138(16) 0.083(5) Uani 1 d . .
H18A H 1.295(10) 0.075(2) -0.179(10) 0.14(5) Uiso 1 calc R .
H18B H 1.369(4) 0.095(4) -0.058(3) 0.14(5) Uiso 1 calc R .
H18C H 1.261(7) 0.115(2) -0.156(12) 0.14(5) Uiso 1 calc R .
C19 C 0.7573(13) 0.0859(4) 0.1331(13) 0.052(3) Uani 1 d . .
H19 H 0.7802(13) 0.1032(4) 0.0670(13) 0.04(3) Uiso 1 calc R .
C20 C 0.6301(14) 0.0995(5) 0.1932(16) 0.074(5) Uani 1 d . .
H20A H 0.604(5) 0.0827(11) 0.257(6) 0.05(2) Uiso 1 calc R .
H20B H 0.555(3) 0.103(2) 0.1255(18) 0.05(2) Uiso 1 calc R .
H20C H 0.651(3) 0.1219(11) 0.235(7) 0.05(2) Uiso 1 calc R .
C21 C 0.7270(19) 0.0503(4) 0.0628(16) 0.079(5) Uani 1 d . .
H21A H 0.807(4) 0.0431(15) 0.020(9) 0.10(4) Uiso 1 calc R .
H21B H 0.649(7) 0.0529(9) -0.001(8) 0.10(4) Uiso 1 calc R .
H21C H 0.707(12) 0.0326(8) 0.126(2) 0.10(4) Uiso 1 calc R .
C22 C 1.1868(13) 0.1401(4) 0.3733(11) 0.051(3) Uani 1 d . .
H22 H 1.1590(13) 0.1584(4) 0.3081(11) 0.01(2) Uiso 1 calc R .
C23 C 1.3307(16) 0.1267(5) 0.345(2) 0.089(6) Uani 1 d . .
H23A H 1.368(4) 0.1116(19) 0.416(5) 0.07(3) Uiso 1 calc R .
H23B H 1.391(3) 0.1466(5) 0.338(9) 0.07(3) Uiso 1 calc R .
H23C H 1.323(2) 0.114(2) 0.265(5) 0.07(3) Uiso 1 calc R .
C24 C 1.189(2) 0.1573(6) 0.5089(16) 0.104(7) Uani 1 d . .
H24A H 1.247(6) 0.1780(12) 0.512(3) 0.05(2) Uiso 1 calc R .
H24B H 1.224(7) 0.1407(9) 0.5748(17) 0.05(2) Uiso 1 calc R .
H24C H 1.096(2) 0.1641(18) 0.524(3) 0.05(2) Uiso 1 calc R .
N3 N 0.9601(7) 0.2135(2) -0.1316(6) 0.044(3) Uani 1 d G .
C25 C 1.0516(7) 0.2117(2) -0.2277(7) 0.047(3) Uani 1 d G .
H25 H 1.1068(11) 0.1917(2) -0.2338(10) 0.060(18) Uiso 1 calc R .
C26 C 1.0607(8) 0.2397(2) -0.3146(7) 0.061(4) Uani 1 d G .
H26 H 1.1219(11) 0.2385(3) -0.3789(9) 0.060(18) Uiso 1 calc R .
C27 C 0.9782(9) 0.2696(2) -0.3055(8) 0.074(5) Uani 1 d G .
H27 H 0.9842(13) 0.2884(3) -0.3636(11) 0.060(18) Uiso 1 calc R .
C28 C 0.8866(9) 0.2715(2) -0.2094(8) 0.055(3) Uani 1 d G .
H28 H 0.8314(12) 0.2915(2) -0.2033(12) 0.060(18) Uiso 1 calc R .
C29 C 0.8776(7) 0.2435(2) -0.1225(7) 0.051(3) Uani 1 d G .
H29 H 0.8163(10) 0.2447(3) -0.0582(9) 0.060(18) Uiso 1 calc R .
N4 N 0.9731(7) 0.2173(2) 0.1688(6) 0.042(2) Uani 1 d G .
C30 C 0.8878(8) 0.2163(2) 0.2701(7) 0.046(3) Uani 1 d G .
H30 H 0.8364(11) 0.1960(2) 0.2835(11) 0.07(2) Uiso 1 calc R .
C31 C 0.8792(8) 0.2456(2) 0.3514(7) 0.063(4) Uani 1 d G .
H31 H 0.8221(12) 0.2449(3) 0.4192(9) 0.07(2) Uiso 1 calc R .
C32 C 0.9560(9) 0.2759(2) 0.3314(8) 0.071(5) Uani 1 d G .
H32 H 0.9503(13) 0.2955(3) 0.3858(11) 0.07(2) Uiso 1 calc R .
C33 C 1.0414(9) 0.2770(2) 0.2301(9) 0.062(4) Uani 1 d G .
H33 H 1.0928(13) 0.2973(2) 0.2167(13) 0.07(2) Uiso 1 calc R .
C34 C 1.0500(8) 0.2477(2) 0.1488(7) 0.056(3) Uani 1 d G .
H34 H 1.1071(11) 0.2484(3) 0.0810(9) 0.07(2) Uiso 1 calc R .
C35 C 0.597(3) -0.0179(8) -0.432(4) 0.138(12) Uani 1 d . .
H35 H 0.668(3) -0.0293(8) -0.380(4) 0.10(5) Uiso 1 calc R .
C36 C 0.593(3) -0.0222(7) -0.557(4) 0.147(13) Uani 1 d . .
H36 H 0.651(3) -0.0377(7) -0.596(4) 0.10(5) Uiso 1 calc R .
C37 C 0.509(3) 0.0014(8) -0.369(4) 0.131(10) Uani 1 d . .
C38 C 0.516(4) 0.0085(9) -0.250(5) 0.093(14) Uani 0.5 d P .
H38A H 0.50(3) -0.0128(17) -0.201(5) 0.16(12) Uiso 0.5 calc PR .
H38B H 0.45(2) 0.025(7) -0.234(6) 0.16(12) Uiso 0.5 calc PR .
H38C H 0.605(13) 0.019(8) -0.222(8) 0.16(12) Uiso 0.5 calc PR .
 
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 0.0252(5) 0.0498(6) 0.0223(5) -0.0003(4) 0.0076(3) -0.0005(4)
Cl1 0.0255(14) 0.072(2) 0.0374(15) 0.0007(13) 0.0093(11) 0.0055(12)
Cl2 0.0263(13) 0.067(2) 0.0334(14) -0.0025(12) 0.0094(11) -0.0065(12)
N1 0.022(4) 0.076(7) 0.024(4) 0.010(4) 0.004(3) 0.006(4)
N2 0.016(4) 0.050(6) 0.031(5) -0.019(4) 0.003(3) -0.009(4)
C1 0.032(6) 0.058(7) 0.023(5) -0.014(5) 0.010(4) -0.013(5)
C2 0.036(6) 0.063(8) 0.028(6) -0.002(5) 0.010(5) -0.007(5)
C3 0.052(8) 0.078(10) 0.042(7) -0.018(7) 0.010(6) -0.013(7)
C4 0.065(9) 0.065(9) 0.054(8) -0.024(7) 0.017(7) -0.009(7)
C5 0.056(8) 0.069(9) 0.042(7) 0.001(6) 0.018(6) 0.003(7)
C6 0.036(6) 0.049(7) 0.040(6) -0.001(5) 0.012(5) 0.009(5)
C7 0.033(6) 0.070(9) 0.031(6) -0.013(6) 0.003(5) -0.011(6)
C8 0.037(9) 0.118(18) 0.21(3) 0.008(17) 0.023(12) 0.003(10)
C9 0.16(2) 0.17(2) 0.075(13) 0.061(14) 0.055(14) 0.092(19)
C10 0.034(6) 0.075(9) 0.020(5) 0.000(5) 0.016(4) 0.010(6)
C11 0.048(7) 0.065(8) 0.032(6) 0.004(6) 0.026(5) 0.003(6)
C12 0.073(10) 0.082(11) 0.064(10) 0.008(8) 0.038(8) -0.007(9)
C13 0.067(10) 0.104(13) 0.048(8) 0.030(8) 0.021(7) 0.014(9)
C14 0.063(9) 0.093(12) 0.039(7) 0.018(7) 0.014(7) 0.030(9)
C15 0.042(7) 0.082(9) 0.025(6) 0.011(6) 0.017(5) 0.020(6)
C16 0.043(7) 0.056(8) 0.048(7) 0.001(6) 0.006(6) 0.010(6)
C17 0.119(16) 0.077(12) 0.071(11) 0.003(9) -0.037(11) 0.024(11)
C18 0.040(8) 0.150(17) 0.061(10) -0.007(10) 0.016(7) 0.002(9)
C19 0.042(7) 0.069(9) 0.048(7) 0.000(6) 0.013(6) -0.015(6)
C20 0.044(8) 0.116(14) 0.065(10) -0.018(9) 0.018(7) -0.006(8)
C21 0.091(12) 0.081(12) 0.069(10) -0.004(9) 0.031(9) -0.030(10)
C22 0.044(7) 0.077(9) 0.031(6) 0.002(6) 0.002(5) 0.021(6)
C23 0.047(9) 0.102(14) 0.119(16) -0.013(12) 0.010(9) 0.010(9)
C24 0.113(16) 0.15(2) 0.049(10) -0.027(11) 0.022(10) -0.017(14)
N3 0.024(5) 0.083(8) 0.027(5) 0.006(5) 0.010(4) 0.002(5)
C25 0.047(7) 0.075(9) 0.020(5) 0.003(5) 0.013(5) 0.002(6)
C26 0.054(8) 0.093(12) 0.037(7) 0.008(7) 0.016(6) -0.009(8)
C27 0.053(9) 0.120(15) 0.050(8) 0.043(9) 0.010(7) -0.005(9)
C28 0.050(8) 0.063(9) 0.052(8) 0.014(7) 0.005(6) 0.007(6)
C29 0.044(7) 0.085(10) 0.025(6) 0.012(6) 0.009(5) 0.009(7)
N4 0.030(5) 0.066(7) 0.030(5) -0.006(4) 0.009(4) 0.001(5)
C30 0.045(7) 0.061(8) 0.032(6) -0.012(5) 0.005(5) 0.006(6)
C31 0.045(8) 0.082(11) 0.062(9) -0.027(8) 0.013(7) 0.001(7)
C32 0.054(9) 0.097(13) 0.062(9) -0.031(9) -0.003(7) 0.017(8)
C33 0.053(8) 0.078(10) 0.055(8) -0.018(7) 0.009(7) -0.006(7)
C34 0.045(7) 0.077(10) 0.048(8) -0.007(7) 0.007(6) -0.003(7)
C35 0.067(15) 0.11(2) 0.23(4) -0.04(2) -0.04(2) -0.001(13)
C36 0.075(16) 0.092(18) 0.27(4) -0.04(3) -0.02(2) -0.005(14)
C37 0.082(16) 0.106(19) 0.20(3) -0.05(2) -0.029(19) -0.031(14)
C38 0.10(3) 0.05(2) 0.13(4) -0.01(2) 0.07(3) -0.03(2)
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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 N2 1.758(9) . ?
Mo1 N1 1.773(10) . ?
Mo1 Cl1 2.395(3) . ?
Mo1 N3 2.396(5) . ?
Mo1 Cl2 2.397(3) . ?
Mo1 N4 2.422(6) . ?
N1 C1 1.374(12) . ?
N2 C10 1.370(11) . ?
C1 C2 1.39 . ?
C1 C6 1.39 . ?
C2 C3 1.39 . ?
C2 C7 1.549(14) . ?
C3 C4 1.39 . ?
C3 H3 0.93 . ?
C4 C5 1.39 . ?
C4 H4 0.93 . ?
C5 C6 1.39 . ?
C5 H5 0.93 . ?
C6 C16 1.525(14) . ?
C7 C9 1.46(2) . ?
C7 C8 1.52(2) . ?
C7 H7 0.98 . ?
C8 H8A 0.96 . ?
C8 H8B 0.96 . ?
C8 H8C 0.96 . ?
C9 H9A 0.96 . ?
C9 H9B 0.96 . ?
C9 H9C 0.96 . ?
C10 C11 1.39 . ?
C10 C15 1.39 . ?
C11 C12 1.39 . ?
C11 C19 1.507(14) . ?
C12 C13 1.39 . ?
C12 H12 0.93 . ?
C13 C14 1.39 . ?
C13 H13 0.93 . ?
C14 C15 1.39 . ?
C14 H14 0.93 . ?
C15 C22 1.53(2) . ?
C16 C18 1.52(2) . ?
C16 C17 1.54(2) . ?
C16 H16 0.98 . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.96 . ?
C18 H18B 0.96 . ?
C18 H18C 0.96 . ?
C19 C20 1.52(2) . ?
C19 C21 1.54(2) . ?
C19 H19 0.98 . ?
C20 H20A 0.96 . ?
C20 H20B 0.96 . ?
C20 H20C 0.96 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 C24 1.53(2) . ?
C22 C23 1.54(2) . ?
C22 H22 0.98 . ?
C23 H23A 0.96 . ?
C23 H23B 0.96 . ?
C23 H23C 0.96 . ?
C24 H24A 0.96 . ?
C24 H24B 0.96 . ?
C24 H24C 0.96 . ?
N3 C25 1.39 . ?
N3 C29 1.39 . ?
C25 C26 1.39 . ?
C25 H25 0.93 . ?
C26 C27 1.39 . ?
C26 H26 0.93 . ?
C27 C28 1.39 . ?
C27 H27 0.93 . ?
C28 C29 1.39 . ?
C28 H28 0.93 . ?
C29 H29 0.93 . ?
N4 C30 1.39 . ?
N4 C34 1.39 . ?
C30 C31 1.39 . ?
C30 H30 0.93 . ?
C31 C32 1.39 . ?
C31 H31 0.93 . ?
C32 C33 1.39 . ?
C32 H32 0.93 . ?
C33 C34 1.39 . ?
C33 H33 0.93 . ?
C34 H34 0.93 . ?
C35 C36 1.29(4) . ?
C35 C37 1.33(4) . ?
C35 H35 0.93 . ?
C36 C37 1.42(4) 3_654 ?
C36 H36 0.93 . ?
C37 C38 1.25(4) . ?
C37 C36 1.42(4) 3_654 ?
C38 H38A 0.96 . ?
C38 H38B 0.96 . ?
C38 H38C 0.9600(13) . ?
 
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
N2 Mo1 N1 102.1(4) . . ?
N2 Mo1 Cl1 96.2(3) . . ?
N1 Mo1 Cl1 96.4(3) . . ?
N2 Mo1 N3 167.8(3) . . ?
N1 Mo1 N3 90.0(4) . . ?
Cl1 Mo1 N3 82.0(2) . . ?
N2 Mo1 Cl2 96.9(3) . . ?
N1 Mo1 Cl2 97.7(3) . . ?
Cl1 Mo1 Cl2 158.37(12) . . ?
N3 Mo1 Cl2 81.6(2) . . ?
N2 Mo1 N4 88.6(3) . . ?
N1 Mo1 N4 169.1(4) . . ?
Cl1 Mo1 N4 80.9(2) . . ?
N3 Mo1 N4 79.2(2) . . ?
Cl2 Mo1 N4 82.2(2) . . ?
C1 N1 Mo1 157.2(7) . . ?
C10 N2 Mo1 166.1(7) . . ?
N1 C1 C2 117.8(6) . . ?
N1 C1 C6 121.9(6) . . ?
C2 C1 C6 120 . . ?
C3 C2 C1 120 . . ?
C3 C2 C7 120.7(6) . . ?
C1 C2 C7 119.2(6) . . ?
C2 C3 C4 120 . . ?
C2 C3 H3 120 . . ?
C4 C3 H3 120 . . ?
C5 C4 C3 120 . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
C4 C5 C6 120 . . ?
C4 C5 H5 120 . . ?
C6 C5 H5 120 . . ?
C5 C6 C1 120 . . ?
C5 C6 C16 119.8(7) . . ?
C1 C6 C16 120.0(7) . . ?
C9 C7 C8 113.5(16) . . ?
C9 C7 C2 110.8(11) . . ?
C8 C7 C2 109.6(12) . . ?
C9 C7 H7 107.6(13) . . ?
C8 C7 H7 107.6(11) . . ?
C2 C7 H7 107.6(5) . . ?
C7 C8 H8A 109.5(11) . . ?
C7 C8 H8B 109.5(11) . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5(10) . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5(12) . . ?
C7 C9 H9B 109.5(12) . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5(9) . . ?
H9A C9 H9C 109.47(7) . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 121.4(6) . . ?
N2 C10 C15 118.5(6) . . ?
C11 C10 C15 120 . . ?
C12 C11 C10 120 . . ?
C12 C11 C19 118.9(7) . . ?
C10 C11 C19 120.8(7) . . ?
C13 C12 C11 120 . . ?
C13 C12 H12 120 . . ?
C11 C12 H12 120 . . ?
C14 C13 C12 120 . . ?
C14 C13 H13 120 . . ?
C12 C13 H13 120 . . ?
C15 C14 C13 120 . . ?
C15 C14 H14 120 . . ?
C13 C14 H14 120 . . ?
C14 C15 C10 120 . . ?
C14 C15 C22 119.4(7) . . ?
C10 C15 C22 120.6(7) . . ?
C18 C16 C6 108.6(10) . . ?
C18 C16 C17 113.1(13) . . ?
C6 C16 C17 112.1(11) . . ?
C18 C16 H16 107.6(9) . . ?
C6 C16 H16 107.6(6) . . ?
C17 C16 H16 107.6(8) . . ?
C16 C17 H17A 109.5(9) . . ?
C16 C17 H17B 109.5(8) . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5(8) . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5(9) . . ?
C16 C18 H18B 109.5(8) . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5(9) . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 C20 110.6(11) . . ?
C11 C19 C21 112.2(12) . . ?
C20 C19 C21 111.0(12) . . ?
C11 C19 H19 107.6(6) . . ?
C20 C19 H19 107.6(9) . . ?
C21 C19 H19 107.6(7) . . ?
C19 C20 H20A 109.5(9) . . ?
C19 C20 H20B 109.5(8) . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5(8) . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5(8) . . ?
C19 C21 H21B 109.5(9) . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5(8) . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C15 112.5(11) . . ?
C24 C22 C23 112.2(14) . . ?
C15 C22 C23 109.9(11) . . ?
C24 C22 H22 107.3(10) . . ?
C15 C22 H22 107.3(5) . . ?
C23 C22 H22 107.3(9) . . ?
C22 C23 H23A 109.5(9) . . ?
C22 C23 H23B 109.5(9) . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5(9) . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5(10) . . ?
C22 C24 H24B 109.5(10) . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5(9) . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 N3 C29 120 . . ?
C25 N3 Mo1 117.3(3) . . ?
C29 N3 Mo1 122.5(3) . . ?
N3 C25 C26 120 . . ?
N3 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C27 C26 C25 120 . . ?
C27 C26 H26 120 . . ?
C25 C26 H26 120 . . ?
C26 C27 C28 120 . . ?
C26 C27 H27 120 . . ?
C28 C27 H27 120 . . ?
C27 C28 C29 120 . . ?
C27 C28 H28 120 . . ?
C29 C28 H28 120 . . ?
C28 C29 N3 120 . . ?
C28 C29 H29 120 . . ?
N3 C29 H29 120 . . ?
C30 N4 C34 120 . . ?
C30 N4 Mo1 116.8(3) . . ?
C34 N4 Mo1 123.1(3) . . ?
C31 C30 N4 120 . . ?
C31 C30 H30 120 . . ?
N4 C30 H30 120 . . ?
C30 C31 C32 120 . . ?
C30 C31 H31 120 . . ?
C32 C31 H31 120 . . ?
C33 C32 C31 120 . . ?
C33 C32 H32 120 . . ?
C31 C32 H32 120 . . ?
C32 C33 C34 120 . . ?
C32 C33 H33 120 . . ?
C34 C33 H33 120 . . ?
C33 C34 N4 120 . . ?
C33 C34 H34 120 . . ?
N4 C34 H34 120 . . ?
C36 C35 C37 126(3) . . ?
C36 C35 H35 117(2) . . ?
C37 C35 H35 117(2) . . ?
C35 C36 C37 114(3) . 3_654 ?
C35 C36 H36 123(2) . . ?
C37 C36 H36 123(3) 3_654 . ?
C38 C37 C35 128(4) . . ?
C38 C37 C36 112(4) . 3_654 ?
C35 C37 C36 120(3) . 3_654 ?
C37 C38 H38A 109(2) . . ?
C37 C38 H38B 110(3) . . ?
H38A C38 H38B 109.47(7) . . ?
C37 C38 H38C 110(2) . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?