#------------------------------------------------------------------------------
#$Date: 2008-01-26 14:05:32 +0100 (Sat, 26 Jan 2008) $
#$Revision: 19 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003087.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2003087
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1999
_journal_volume     B55
_journal_page_first     410
_journal_page_last     423
;
Frederik C. Krebs
;
_chemical_name_systematic
;
 Bis(2,6,10-tri-tert-butyl-4,8,12-trioxa-4,8,12,12c-tetrahydro-
dibenzo[cd,mn]pyrenium) tetradecachlorohexamolybdate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C31 H33 O3,Cl7 Mo3'
_chemical_formula_sum     'C31 H33 Cl7 Mo3 O3'
_chemical_formula_weight     989.54
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/n'
_symmetry_space_group_name_Hall     '-P 2yn'
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     17.157(3)
_cell_length_b     11.130(2)
_cell_length_c     18.456(4)
_cell_angle_alpha     90.00
_cell_angle_beta     96.40(3)
_cell_angle_gamma     90.00
_cell_volume     3502.4(12)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min     ?
_cell_measurement_theta_max     ?
_cell_measurement_temperature     120(2)
_exptl_crystal_description     cube
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.28
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.20
_exptl_crystal_density_diffrn     1.877
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1952
_exptl_absorpt_coefficient_mu     1.624
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_correction_T_min     0.704
_exptl_absorpt_correction_T_max     0.886
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens SMART CCD'
_diffrn_measurement_method     'omega scan, frame data integration'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     36072
_diffrn_reflns_av_R_equivalents     0.0271
_diffrn_reflns_av_sigmaI/netI     0.0197
_diffrn_reflns_theta_min     1.54
_diffrn_reflns_theta_max     26.37
_diffrn_reflns_theta_full     26.37
_diffrn_measured_fraction_theta_max     0.948
_diffrn_measured_fraction_theta_full     0.948
_diffrn_reflns_limit_h_min     -21
_diffrn_reflns_limit_h_max     21
_diffrn_reflns_limit_k_min     -13
_diffrn_reflns_limit_k_max     13
_diffrn_reflns_limit_l_min     -23
_diffrn_reflns_limit_l_max     23
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_reflns_number_total     7149
_reflns_number_gt     6258
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0294
_refine_ls_R_factor_gt     0.0234
_refine_ls_wR_factor_ref     0.0582
_refine_ls_goodness_of_fit_ref     1.097
_refine_ls_restrained_S_all     1.097
_refine_ls_number_reflns     7149
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme
         'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.6569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_shift/su_max     0.005
_refine_diff_density_max     0.434
_refine_diff_density_min     -1.313
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         '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'
    '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_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Mo1 0.950784(10) 0.876155(17) 0.043899(10) 0.01156(5) Uani d . 1 . . Mo
    Mo2 1.014830(10) 1.079316(17) 0.088032(10) 0.01214(5) Uani d . 1 . . Mo
    Mo3 1.095215(10) 0.923207(17) 0.021136(10) 0.01187(5) Uani d . 1 . . Mo
    Cl1 0.88433(3) 0.71653(5) 0.10371(3) 0.02044(12) Uani d . 1 . . Cl
    Cl2 1.03377(4) 1.17836(6) 0.20545(3) 0.02654(14) Uani d . 1 . . Cl
    Cl3 1.22017(3) 0.81908(5) 0.04631(3) 0.02215(13) Uani d . 1 . . Cl
    Cl4 0.87735(3) 1.03036(5) 0.10448(3) 0.01702(12) Uani d . 1 . . Cl
    Cl5 1.15006(3) 1.12096(5) 0.06237(3) 0.01617(11) Uani d . 1 . . Cl
    Cl6 1.02882(3) 0.73467(5) -0.02202(3) 0.01627(11) Uani d . 1 . . Cl
    Cl7 1.05821(3) 0.88635(5) 0.14517(3) 0.01713(11) Uani d . 1 . . Cl
    O1 0.45707(8) 0.82772(14) -0.15806(8) 0.0135(3) Uani d . 1 . . O
    O2 0.31766(8) 1.08819(14) -0.00779(8) 0.0139(3) Uani d . 1 . . O
    O3 0.49862(8) 0.79292(14) 0.10404(8) 0.0143(3) Uani d . 1 . . O
    C1 0.42274(12) 0.90108(19) -0.02062(12) 0.0116(4) Uani d . 1 . . C
    C2 0.38625(12) 0.9570(2) -0.08306(12) 0.0126(4) Uani d . 1 . . C
    C3 0.40530(12) 0.92167(19) -0.15203(12) 0.0130(4) Uani d . 1 . . C
    C4 0.37376(12) 0.9821(2) -0.21344(11) 0.0140(4) Uani d . 1 . . C
    H4 0.3863 0.9595 -0.2592 0.017 Uiso calc . 1 . . H
    C5 0.32230(12) 1.0787(2) -0.20608(12) 0.0136(4) Uani d . 1 . . C
    C6 0.30081(12) 1.1120(2) -0.13717(12) 0.0147(4) Uani d . 1 . . C
    H6 0.2648 1.1734 -0.1331 0.018 Uiso calc . 1 . . H
    C7 0.33425(12) 1.0517(2) -0.07596(12) 0.0132(4) Uani d . 1 . . C
    C8 0.40717(12) 0.93901(19) 0.04778(12) 0.0121(4) Uani d . 1 . . C
    C9 0.35416(12) 1.0337(2) 0.05407(12) 0.0130(4) Uani d . 1 . . C
    C10 0.33960(12) 1.07279(19) 0.12195(12) 0.0137(4) Uani d . 1 . . C
    H10 0.3059 1.1371 0.1264 0.016 Uiso calc . 1 . . H
    C11 0.37588(12) 1.01525(19) 0.18422(12) 0.0128(4) Uani d . 1 . . C
    C12 0.42924(12) 0.9201(2) 0.17862(12) 0.0137(4) Uani d . 1 . . C
    H12 0.4534 0.8827 0.2203 0.016 Uiso calc . 1 . . H
    C13 0.44492(12) 0.88392(19) 0.11086(12) 0.0124(4) Uani d . 1 . . C
    C14 0.47708(12) 0.80968(19) -0.02700(11) 0.0125(4) Uani d . 1 . . C
    C15 0.51501(12) 0.75612(19) 0.03610(11) 0.0123(4) Uani d . 1 . . C
    C16 0.56837(12) 0.6654(2) 0.02997(12) 0.0138(4) Uani d . 1 . . C
    H16 0.5941 0.6300 0.0716 0.017 Uiso calc . 1 . . H
    C17 0.58391(12) 0.62647(19) -0.03938(12) 0.0134(4) Uani d . 1 . . C
    C18 0.54567(12) 0.6798(2) -0.10273(12) 0.0137(4) Uani d . 1 . . C
    H18 0.5557 0.6531 -0.1485 0.016 Uiso calc . 1 . . H
    C19 0.49324(12) 0.7719(2) -0.09639(11) 0.0127(4) Uani d . 1 . . C
    C20 0.28787(13) 1.1522(2) -0.27219(12) 0.0168(5) Uani d . 1 . . C
    C21 0.19862(14) 1.1307(2) -0.28355(13) 0.0215(5) Uani d . 1 . . C
    H21A 0.1763 1.1509 -0.2397 0.032 Uiso calc . 1 . . H
    H21B 0.1885 1.0476 -0.2951 0.032 Uiso calc . 1 . . H
    H21C 0.1756 1.1800 -0.3229 0.032 Uiso calc . 1 . . H
    C22 0.32445(14) 1.1189(2) -0.34166(13) 0.0232(5) Uani d . 1 . . C
    H22A 0.3800 1.1323 -0.3341 0.035 Uiso calc . 1 . . H
    H22B 0.3018 1.1677 -0.3814 0.035 Uiso calc . 1 . . H
    H22C 0.3144 1.0357 -0.3529 0.035 Uiso calc . 1 . . H
    C23 0.30369(15) 1.2866(2) -0.25642(13) 0.0236(5) Uani d . 1 . . C
    H23A 0.3592 1.3005 -0.2491 0.035 Uiso calc . 1 . . H
    H23B 0.2807 1.3095 -0.2134 0.035 Uiso calc . 1 . . H
    H23C 0.2810 1.3336 -0.2970 0.035 Uiso calc . 1 . . H
    C24 0.35515(13) 1.0489(2) 0.26010(12) 0.0171(5) Uani d . 1 . . C
    C25 0.30681(14) 1.1646(2) 0.25967(13) 0.0229(5) Uani d . 1 . . C
    H25A 0.2602 1.1562 0.2261 0.034 Uiso calc . 1 . . H
    H25B 0.3374 1.2307 0.2450 0.034 Uiso calc . 1 . . H
    H25C 0.2925 1.1794 0.3077 0.034 Uiso calc . 1 . . H
    C26 0.43001(16) 1.0650(3) 0.31308(14) 0.0298(6) Uani d . 1 . . C
    H26A 0.4161 1.0855 0.3605 0.045 Uiso calc . 1 . . H
    H26B 0.4613 1.1281 0.2958 0.045 Uiso calc . 1 . . H
    H26C 0.4594 0.9914 0.3160 0.045 Uiso calc . 1 . . H
    C27 0.30638(18) 0.9441(3) 0.28503(16) 0.0346(7) Uani d . 1 . . C
    H27A 0.2600 0.9342 0.2514 0.052 Uiso calc . 1 . . H
    H27B 0.2918 0.9609 0.3327 0.052 Uiso calc . 1 . . H
    H27C 0.3369 0.8716 0.2866 0.052 Uiso calc . 1 . . H
    C28 0.64667(12) 0.5300(2) -0.04476(12) 0.0143(4) Uani d . 1 . . C
    C29 0.63263(14) 0.4595(2) -0.11678(13) 0.0203(5) Uani d . 1 . . C
    H29A 0.6328 0.5140 -0.1571 0.031 Uiso calc . 1 . . H
    H29B 0.5828 0.4195 -0.1195 0.031 Uiso calc . 1 . . H
    H29C 0.6735 0.4010 -0.1187 0.031 Uiso calc . 1 . . H
    C30 0.72640(14) 0.5947(2) -0.03938(14) 0.0228(5) Uani d . 1 . . C
    H30A 0.7344 0.6384 0.0057 0.034 Uiso calc . 1 . . H
    H30B 0.7270 0.6495 -0.0795 0.034 Uiso calc . 1 . . H
    H30C 0.7675 0.5366 -0.0410 0.034 Uiso calc . 1 . . H
    C31 0.64836(14) 0.4411(2) 0.01860(14) 0.0219(5) Uani d . 1 . . C
    H31A 0.6552 0.4841 0.0639 0.033 Uiso calc . 1 . . H
    H31B 0.6911 0.3860 0.0166 0.033 Uiso calc . 1 . . H
    H31C 0.5999 0.3973 0.0150 0.033 Uiso calc . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Mo1 0.01039(9) 0.01106(10) 0.01335(10) -0.00042(7) 0.00189(7) -0.00083(7)
    Mo2 0.01238(9) 0.01202(10) 0.01198(10) -0.00028(7) 0.00120(7) -0.00290(7)
    Mo3 0.00936(9) 0.01110(10) 0.01507(10) 0.00076(7) 0.00105(7) -0.00121(7)
    Cl1 0.0187(3) 0.0178(3) 0.0252(3) -0.0031(2) 0.0044(2) 0.0046(2)
    Cl2 0.0354(3) 0.0265(3) 0.0173(3) -0.0032(3) 0.0011(2) -0.0103(2)
    Cl3 0.0127(2) 0.0180(3) 0.0352(3) 0.0039(2) 0.0003(2) 0.0011(2)
    Cl4 0.0158(3) 0.0175(3) 0.0190(3) 0.0003(2) 0.0074(2) -0.0028(2)
    Cl5 0.0120(2) 0.0156(3) 0.0203(3) -0.00195(19) -0.0012(2) -0.0021(2)
    Cl6 0.0158(2) 0.0117(3) 0.0215(3) 0.0010(2) 0.0030(2) -0.0031(2)
    Cl7 0.0182(3) 0.0174(3) 0.0150(3) 0.0000(2) -0.0013(2) 0.0017(2)
    O1 0.0156(7) 0.0132(8) 0.0118(7) 0.0033(6) 0.0023(6) 0.0004(6)
    O2 0.0133(7) 0.0150(8) 0.0137(8) 0.0036(6) 0.0032(6) 0.0012(6)
    O3 0.0161(7) 0.0145(8) 0.0126(7) 0.0042(6) 0.0032(6) 0.0008(6)
    C1 0.0097(9) 0.0091(10) 0.0162(11) -0.0030(8) 0.0027(8) -0.0001(8)
    C2 0.0105(10) 0.0121(11) 0.0154(11) -0.0002(8) 0.0021(8) 0.0020(8)
    C3 0.0103(10) 0.0118(11) 0.0169(11) -0.0009(8) 0.0022(8) 0.0000(9)
    C4 0.0139(10) 0.0162(12) 0.0121(10) -0.0013(9) 0.0028(8) -0.0003(9)
    C5 0.0114(10) 0.0131(11) 0.0161(11) -0.0019(8) 0.0012(8) 0.0023(9)
    C6 0.0125(10) 0.0127(11) 0.0190(11) 0.0019(8) 0.0028(9) 0.0015(9)
    C7 0.0110(10) 0.0143(11) 0.0144(11) -0.0019(8) 0.0027(8) -0.0011(9)
    C8 0.0112(10) 0.0113(11) 0.0143(11) -0.0015(8) 0.0033(8) 0.0002(8)
    C9 0.0113(10) 0.0130(11) 0.0146(11) -0.0015(8) 0.0016(8) 0.0016(9)
    C10 0.0103(10) 0.0127(11) 0.0184(11) -0.0018(8) 0.0035(8) -0.0027(9)
    C11 0.0115(10) 0.0123(11) 0.0154(11) -0.0053(8) 0.0048(8) -0.0032(9)
    C12 0.0147(10) 0.0134(11) 0.0130(11) -0.0020(8) 0.0013(8) 0.0022(9)
    C13 0.0115(10) 0.0091(11) 0.0171(11) 0.0007(8) 0.0034(8) 0.0016(8)
    C14 0.0119(10) 0.0103(10) 0.0159(11) -0.0012(8) 0.0039(8) -0.0013(8)
    C15 0.0121(10) 0.0118(11) 0.0136(10) -0.0010(8) 0.0040(8) -0.0012(8)
    C16 0.0146(10) 0.0127(11) 0.0139(10) 0.0010(8) 0.0004(8) 0.0020(9)
    C17 0.0114(10) 0.0105(11) 0.0189(11) -0.0021(8) 0.0042(8) -0.0003(9)
    C18 0.0141(10) 0.0135(11) 0.0142(10) -0.0017(8) 0.0043(8) -0.0013(9)
    C19 0.0112(10) 0.0123(11) 0.0149(11) -0.0013(8) 0.0034(8) 0.0027(8)
    C20 0.0176(11) 0.0172(12) 0.0156(11) 0.0029(9) 0.0016(9) 0.0040(9)
    C21 0.0189(11) 0.0254(13) 0.0196(12) 0.0044(10) -0.0012(9) 0.0028(10)
    C22 0.0258(13) 0.0279(14) 0.0164(12) 0.0089(10) 0.0045(10) 0.0060(10)
    C23 0.0294(13) 0.0188(13) 0.0230(13) 0.0021(10) 0.0045(10) 0.0064(10)
    C24 0.0198(11) 0.0175(12) 0.0148(11) 0.0011(9) 0.0057(9) -0.0022(9)
    C25 0.0251(12) 0.0258(14) 0.0183(12) 0.0067(10) 0.0046(10) -0.0060(10)
    C26 0.0329(14) 0.0376(16) 0.0172(12) 0.0143(12) -0.0046(11) -0.0106(11)
    C27 0.0465(17) 0.0268(15) 0.0362(16) -0.0020(12) 0.0301(13) 0.0022(12)
    C28 0.0131(10) 0.0135(11) 0.0163(11) 0.0019(9) 0.0023(8) -0.0015(9)
    C29 0.0212(11) 0.0178(12) 0.0220(12) 0.0061(10) 0.0023(9) -0.0040(10)
    C30 0.0147(11) 0.0234(13) 0.0313(14) -0.0009(10) 0.0064(10) -0.0058(11)
    C31 0.0251(12) 0.0162(12) 0.0255(13) 0.0073(10) 0.0073(10) 0.0025(10)