#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321499.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_4321499
loop_
_publ_author_name
'Andrew J. Millar'
'Jonathan M. White'
'Christian J. Doonan'
'Charles G. Young'
_publ_section_title
;
 Synthesis and Characterization of Monomeric Oxo Dichloro 1,3-Dialkyl
 p-tert-Butylcalix[4]arene Complexes of Molybdenum(VI,V) and
 Tungsten(VI,V)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5151
_journal_page_last               5155
_journal_paper_doi               10.1021/ic000431i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C49 H63 Cl5 Mo O5'
_chemical_formula_weight         1005.18
_chemical_name_systematic
; 
(1,3-dimethyl tetra-p-tert-butylcalix[4]arene-O1,O2,O4)dichlorooxomolybdenum(VI)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.87(2)
_cell_angle_beta                 112.00(2)
_cell_angle_gamma                112.090(10)
_cell_formula_units_Z            2
_cell_length_a                   13.230(3)
_cell_length_b                   14.950(3)
_cell_length_c                   15.799(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     2574.9(12)
_computing_data_reduction        Process-Data
_computing_molecular_graphics    ZORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Enraf Nonius'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9132
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  9600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.556
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         8703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.255
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0725P)²+2.1545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                6943
_reflns_number_total             8703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000431i_1.cif
_cod_data_source_block           jmwcd1
_cod_original_cell_volume        2574.9(10)
_cod_database_code               4321499
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.27635(3) 0.02335(2) 0.76589(2) 0.03961(13) Uani 1 1 d . . .
Cl1 Cl 0.06039(9) -0.03528(8) 0.68301(7) 0.0577(3) Uani 1 1 d . . .
Cl2 Cl 0.23769(11) -0.14789(8) 0.72330(9) 0.0641(3) Uani 1 1 d . . .
Cl3 Cl 0.02059(19) 0.68377(16) 0.82153(13) 0.1159(6) Uani 1 1 d . . .
Cl4 Cl -0.0976(3) 0.64497(17) 0.62170(14) 0.1566(10) Uani 1 1 d . . .
Cl5 Cl -0.1668(2) 0.7425(2) 0.7392(2) 0.1700(11) Uani 1 1 d . . .
O1 O 0.2507(2) 0.00113(18) 0.60713(16) 0.0417(6) Uani 1 1 d . . .
O2 O 0.4396(2) 0.06016(18) 0.79591(17) 0.0437(6) Uani 1 1 d . . .
O3 O 0.4349(3) 0.1746(2) 1.01789(18) 0.0543(7) Uani 1 1 d . . .
O4 O 0.2883(2) 0.15123(18) 0.75862(17) 0.0416(6) Uani 1 1 d . . .
O5 O 0.2741(3) 0.0187(2) 0.86908(19) 0.0547(7) Uani 1 1 d . . .
C1 C 0.3317(3) 0.0826(3) 0.5910(2) 0.0380(8) Uani 1 1 d . . .
C2 C 0.2990(3) 0.1581(3) 0.5674(2) 0.0387(8) Uani 1 1 d . . .
C3 C 0.3775(3) 0.2347(3) 0.5460(3) 0.0451(9) Uani 1 1 d . . .
H3 H 0.3570 0.2854 0.5286 0.054 Uiso 1 1 calc R . .
C4 C 0.4857(3) 0.2375(3) 0.5497(3) 0.0456(9) Uani 1 1 d . . .
C5 C 0.5168(3) 0.1636(3) 0.5801(3) 0.0436(9) Uani 1 1 d . . .
H5 H 0.5908 0.1663 0.5864 0.052 Uiso 1 1 calc R . .
C6 C 0.4408(3) 0.0852(3) 0.6014(2) 0.0391(8) Uani 1 1 d . . .
C7 C 0.4785(3) 0.0064(3) 0.6360(3) 0.0444(9) Uani 1 1 d . . .
H7A H 0.4072 -0.0506 0.6303 0.053 Uiso 1 1 calc R . .
H7B H 0.5080 -0.0170 0.5951 0.053 Uiso 1 1 calc R . .
C8 C 0.5762(3) 0.0442(3) 0.7378(3) 0.0411(8) Uani 1 1 d . . .
C9 C 0.6920(4) 0.0563(3) 0.7586(3) 0.0503(9) Uani 1 1 d . . .
H10 H 0.7089 0.0408 0.7085 0.060 Uiso 1 1 calc R . .
C10 C 0.7858(4) 0.0908(3) 0.8514(3) 0.0519(10) Uani 1 1 d . . .
C11 C 0.7568(4) 0.1113(3) 0.9242(3) 0.0522(10) Uani 1 1 d . . .
H12 H 0.8171 0.1327 0.9866 0.063 Uiso 1 1 calc R . .
C12 C 0.6423(3) 0.1016(3) 0.9091(3) 0.0447(9) Uani 1 1 d . . .
C13 C 0.5517(3) 0.0675(3) 0.8142(3) 0.0404(8) Uani 1 1 d . . .
C14 C 0.6209(4) 0.1376(3) 0.9906(3) 0.0496(9) Uani 1 1 d . . .
H14A H 0.6897 0.1518 1.0507 0.059 Uiso 1 1 calc R . .
H14B H 0.5482 0.0859 0.9889 0.059 Uiso 1 1 calc R . .
C15 C 0.6053(3) 0.2327(3) 0.9817(2) 0.0433(9) Uani 1 1 d . . .
C16 C 0.6784(3) 0.3057(3) 0.9547(3) 0.0483(9) Uani 1 1 d . . .
H17 H 0.7485 0.3035 0.9566 0.058 Uiso 1 1 calc R . .
C17 C 0.6522(4) 0.3820(3) 0.9249(3) 0.0494(9) Uani 1 1 d . . .
C18 C 0.5445(4) 0.3801(3) 0.9190(3) 0.0495(9) Uani 1 1 d . . .
H19 H 0.5219 0.4279 0.8960 0.059 Uiso 1 1 calc R . .
C19 C 0.4686(3) 0.3089(3) 0.9462(2) 0.0450(9) Uani 1 1 d . . .
C20 C 0.5059(3) 0.2411(3) 0.9851(2) 0.0426(8) Uani 1 1 d . . .
C21 C 0.3398(4) 0.2958(3) 0.9215(3) 0.0519(10) Uani 1 1 d . . .
H21A H 0.2930 0.2323 0.9294 0.062 Uiso 1 1 calc R . .
H21B H 0.3438 0.3495 0.9646 0.062 Uiso 1 1 calc R . .
C22 C 0.2770(3) 0.2976(3) 0.8204(3) 0.0431(8) Uani 1 1 d . . .
C23 C 0.2444(4) 0.3732(3) 0.8022(3) 0.0503(10) Uani 1 1 d . . .
H24 H 0.2581 0.4207 0.8533 0.060 Uiso 1 1 calc R . .
C24 C 0.1914(4) 0.3821(3) 0.7105(3) 0.0480(9) Uani 1 1 d . . .
C25 C 0.1738(3) 0.3111(3) 0.6364(3) 0.0450(9) Uani 1 1 d . . .
H26 H 0.1391 0.3155 0.5747 0.054 Uiso 1 1 calc R . .
C26 C 0.2056(3) 0.2334(3) 0.6499(2) 0.0396(8) Uani 1 1 d . . .
C27 C 0.2555(3) 0.2260(3) 0.7428(2) 0.0382(8) Uani 1 1 d . . .
C28 C 0.1837(3) 0.1589(3) 0.5654(2) 0.0438(9) Uani 1 1 d . . .
H28A H 0.1425 0.1742 0.5078 0.053 Uiso 1 1 calc R . .
H28B H 0.1296 0.0921 0.5624 0.053 Uiso 1 1 calc R . .
C29 C 0.5617(4) 0.3154(3) 0.5139(3) 0.0606(11) Uani 1 1 d . . .
C30 C 0.6928(5) 0.3342(5) 0.5560(6) 0.109(2) Uani 1 1 d . . .
H30A H 0.7298 0.3616 0.6238 0.163 Uiso 1 1 calc R . .
H30B H 0.7357 0.3810 0.5297 0.163 Uiso 1 1 calc R . .
H30C H 0.6965 0.2719 0.5413 0.163 Uiso 1 1 calc R . .
C31 C 0.497(5) 0.303(9) 0.413(2) 0.15(3) Uani 0.47(14) 1 d P . .
C31' C 0.507(3) 0.256(4) 0.403(2) 0.123(9) Uani 0.53(14) 1 d P . .
C32 C 0.5634(8) 0.4151(5) 0.5408(8) 0.161(4) Uani 1 1 d . . .
H32A H 0.5993 0.4395 0.6089 0.241 Uiso 1 1 calc R . .
H32B H 0.4815 0.4076 0.5136 0.241 Uiso 1 1 calc R . .
H32C H 0.6107 0.4622 0.5173 0.241 Uiso 1 1 calc R . .
C33 C 0.9133(4) 0.1055(5) 0.8686(4) 0.0752(14) Uani 1 1 d . . .
C34 C 1.0027(6) 0.1451(7) 0.9739(5) 0.135(3) Uani 1 1 d . . .
H34A H 1.0814 0.1530 0.9815 0.202 Uiso 1 1 calc R . .
H34B H 0.9740 0.0983 1.0066 0.202 Uiso 1 1 calc R . .
H34C H 1.0093 0.2090 1.0001 0.202 Uiso 1 1 calc R . .
C35 C 0.9629(6) 0.1827(8) 0.8215(7) 0.171(5) Uani 1 1 d . . .
H35A H 1.0428 0.1919 0.8319 0.257 Uiso 1 1 calc R . .
H35B H 0.9675 0.2456 0.8484 0.257 Uiso 1 1 calc R . .
H35C H 0.9097 0.1597 0.7544 0.257 Uiso 1 1 calc R . .
C36 C 0.9047(7) 0.0048(7) 0.8281(6) 0.145(3) Uani 1 1 d . . .
H36A H 0.9843 0.0130 0.8383 0.217 Uiso 1 1 calc R . .
H36B H 0.8510 -0.0196 0.7610 0.217 Uiso 1 1 calc R . .
H36C H 0.8734 -0.0427 0.8593 0.217 Uiso 1 1 calc R . .
C37 C 0.7367(4) 0.4597(3) 0.8951(3) 0.0636(12) Uani 1 1 d . . .
C38 C 0.7700(8) 0.4083(5) 0.8307(5) 0.124(3) Uani 1 1 d . . .
H38A H 0.8068 0.3690 0.8621 0.186 Uiso 1 1 calc R . .
H38B H 0.8266 0.4579 0.8156 0.186 Uiso 1 1 calc R . .
H38C H 0.6978 0.3650 0.7732 0.186 Uiso 1 1 calc R . .
C39 C 0.8515(7) 0.5322(5) 0.9833(5) 0.142(3) Uani 1 1 d . . .
H39A H 0.8304 0.5651 1.0247 0.213 Uiso 1 1 calc R . .
H39B H 0.9046 0.5816 0.9654 0.213 Uiso 1 1 calc R . .
H39C H 0.8924 0.4959 1.0159 0.213 Uiso 1 1 calc R . .
C40 C 0.6806(9) 0.5216(7) 0.8467(8) 0.169(4) Uani 1 1 d . . .
H40A H 0.6605 0.5554 0.8883 0.253 Uiso 1 1 calc R . .
H40B H 0.6078 0.4787 0.7894 0.253 Uiso 1 1 calc R . .
H40C H 0.7374 0.5706 0.8311 0.253 Uiso 1 1 calc R . .
C41 C 0.1558(5) 0.4682(4) 0.6933(3) 0.0695(13) Uani 1 1 d . . .
C42 C 0.186(4) 0.546(2) 0.7823(18) 0.119(11) Uani 0.46(8) 1 d P . .
C42' C 0.236(5) 0.5574(15) 0.770(3) 0.173(17) Uani 0.54(8) 1 d P . .
C43 C 0.2343(17) 0.5307(9) 0.6437(11) 0.120(8) Uani 0.61(2) 1 d P . .
C43' C 0.092(3) 0.4629(16) 0.5921(14) 0.126(14) Uani 0.39(2) 1 d P . .
C44 C 0.0357(16) 0.4351(13) 0.7249(17) 0.079(8) Uani 0.34(2) 1 d P . .
C44' C 0.0264(12) 0.4261(9) 0.6229(16) 0.149(11) Uani 0.66(2) 1 d P . .
C45 C 0.1494(4) -0.0771(3) 0.5197(3) 0.0616(12) Uani 1 1 d . . .
H45A H 0.0915 -0.1238 0.5369 0.074 Uiso 1 1 calc R . .
H45B H 0.1078 -0.0453 0.4788 0.074 Uiso 1 1 calc R . .
C46 C 0.1838(5) -0.1328(5) 0.4668(4) 0.115(3) Uani 1 1 d . . .
H46A H 0.1126 -0.1812 0.4112 0.173 Uiso 1 1 calc R . .
H46B H 0.2223 -0.1669 0.5056 0.173 Uiso 1 1 calc R . .
H46C H 0.2398 -0.0877 0.4480 0.173 Uiso 1 1 calc R . .
C47 C 0.4748(7) 0.1945(7) 1.1157(4) 0.142(4) Uani 1 1 d . . .
C48 C 0.3857(16) 0.1678(16) 1.1450(10) 0.140(7) Uani 0.63(3) 1 d P . .
C48' C 0.419(2) 0.250(3) 1.1485(13) 0.109(13) Uani 0.37(3) 1 d P . .
C49 C -0.0489(5) 0.7263(4) 0.7289(4) 0.0802(15) Uani 1 1 d . . .
H49 H 0.0119 0.7919 0.7336 0.096 Uiso 1 1 calc R . .
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_
_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
O5 Mo O2 102.55(13) . . ?
O5 Mo O4 103.38(13) . . ?
O2 Mo O4 94.38(11) . . ?
O5 Mo O1 169.91(12) . . ?
O2 Mo O1 83.76(10) . . ?
O4 Mo O1 83.76(10) . . ?
O5 Mo Cl2 93.20(11) . . ?
O2 Mo Cl2 88.07(8) . . ?
O4 Mo Cl2 162.25(8) . . ?
O1 Mo Cl2 79.03(7) . . ?
O5 Mo Cl1 93.00(11) . . ?
O2 Mo Cl1 163.93(8) . . ?
O4 Mo Cl1 85.80(8) . . ?
O1 Mo Cl1 80.29(7) . . ?
Cl2 Mo Cl1 87.05(5) . . ?
C1 O1 C45 114.3(3) . . ?
C1 O1 Mo 115.52(18) . . ?
C45 O1 Mo 129.2(2) . . ?
C13 O2 Mo 168.9(2) . . ?
C20 O3 C47 117.8(4) . . ?
C27 O4 Mo 160.5(2) . . ?
C6 C1 C2 122.9(3) . . ?
C6 C1 O1 118.6(3) . . ?
C2 C1 O1 118.5(3) . . ?
C1 C2 C3 117.2(3) . . ?
C1 C2 C28 122.1(3) . . ?
C3 C2 C28 120.8(3) . . ?
C4 C3 C2 122.1(4) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 117.7(3) . . ?
C5 C4 C29 121.7(4) . . ?
C3 C4 C29 120.5(4) . . ?
C4 C5 C6 122.2(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 117.7(3) . . ?
C1 C6 C7 121.4(3) . . ?
C5 C6 C7 120.9(3) . . ?
C8 C7 C6 113.7(3) . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 117.8(3) . . ?
C9 C8 C7 120.9(3) . . ?
C13 C8 C7 121.3(3) . . ?
C8 C9 C10 123.3(4) . . ?
C8 C9 H10 118.4 . . ?
C10 C9 H10 118.4 . . ?
C11 C10 C9 116.8(4) . . ?
C11 C10 C33 123.1(4) . . ?
C9 C10 C33 120.2(4) . . ?
C10 C11 C12 123.4(4) . . ?
C10 C11 H12 118.3 . . ?
C12 C11 H12 118.3 . . ?
C11 C12 C13 117.4(4) . . ?
C11 C12 C14 120.8(4) . . ?
C13 C12 C14 121.4(3) . . ?
O2 C13 C8 119.3(3) . . ?
O2 C13 C12 119.4(3) . . ?
C8 C13 C12 121.3(3) . . ?
C12 C14 C15 108.8(3) . . ?
C12 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
C12 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C16 C15 C20 117.7(4) . . ?
C16 C15 C14 120.6(3) . . ?
C20 C15 C14 120.8(3) . . ?
C15 C16 C17 123.2(4) . . ?
C15 C16 H17 118.4 . . ?
C17 C16 H17 118.4 . . ?
C18 C17 C16 116.6(4) . . ?
C18 C17 C37 122.9(4) . . ?
C16 C17 C37 120.4(4) . . ?
C17 C18 C19 122.2(4) . . ?
C17 C18 H19 118.9 . . ?
C19 C18 H19 118.9 . . ?
C20 C19 C18 118.7(4) . . ?
C20 C19 C21 119.9(4) . . ?
C18 C19 C21 120.9(4) . . ?
O3 C20 C15 120.3(3) . . ?
O3 C20 C19 118.9(3) . . ?
C15 C20 C19 120.4(3) . . ?
C22 C21 C19 110.8(3) . . ?
C22 C21 H21A 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C23 C22 C27 118.0(3) . . ?
C23 C22 C21 120.2(3) . . ?
C27 C22 C21 121.7(3) . . ?
C22 C23 C24 123.1(4) . . ?
C22 C23 H24 118.4 . . ?
C24 C23 H24 118.4 . . ?
C25 C24 C23 116.9(4) . . ?
C25 C24 C41 121.6(4) . . ?
C23 C24 C41 121.4(4) . . ?
C24 C25 C26 122.8(3) . . ?
C24 C25 H26 118.6 . . ?
C26 C25 H26 118.6 . . ?
C25 C26 C27 118.2(3) . . ?
C25 C26 C28 119.7(3) . . ?
C27 C26 C28 122.0(3) . . ?
O4 C27 C26 119.8(3) . . ?
O4 C27 C22 119.3(3) . . ?
C26 C27 C22 120.8(3) . . ?
C26 C28 C2 114.2(3) . . ?
C26 C28 H28A 108.7 . . ?
C2 C28 H28A 108.7 . . ?
C26 C28 H28B 108.7 . . ?
C2 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C31 C29 C32 92(6) . . ?
C31 C29 C30 120(4) . . ?
C32 C29 C30 106.2(5) . . ?
C31 C29 C4 113.0(16) . . ?
C32 C29 C4 111.0(4) . . ?
C30 C29 C4 112.4(4) . . ?
C31 C29 C31' 29(5) . . ?
C32 C29 C31' 121(2) . . ?
C30 C29 C31' 103.7(14) . . ?
C4 C29 C31' 102.5(14) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31' C31 C29 87(8) . . ?
C31 C31' C29 64(4) . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C36 111.1(7) . . ?
C35 C33 C34 106.9(6) . . ?
C36 C33 C34 108.8(6) . . ?
C35 C33 C10 109.2(5) . . ?
C36 C33 C10 108.6(5) . . ?
C34 C33 C10 112.2(4) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C40 C37 C38 109.5(6) . . ?
C40 C37 C39 106.5(6) . . ?
C38 C37 C39 109.3(6) . . ?
C40 C37 C17 112.2(4) . . ?
C38 C37 C17 110.3(4) . . ?
C39 C37 C17 108.9(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42' C41 C44' 133(2) . . ?
C42' C41 C43' 126.1(19) . . ?
C44' C41 C43' 45.6(14) . . ?
C42' C41 C24 111.8(10) . . ?
C44' C41 C24 109.8(6) . . ?
C43' C41 C24 114.9(9) . . ?
C42' C41 C42 28(3) . . ?
C44' C41 C42 111.8(18) . . ?
C43' C41 C42 128.5(14) . . ?
C24 C41 C42 116.6(11) . . ?
C42' C41 C43 82(3) . . ?
C44' C41 C43 106.2(12) . . ?
C43' C41 C43 61.0(13) . . ?
C24 C41 C43 106.0(5) . . ?
C42 C41 C43 105.7(16) . . ?
C42' C41 C44 95(3) . . ?
C44' C41 C44 56.9(10) . . ?
C43' C41 C44 101.2(16) . . ?
C24 C41 C44 100.7(6) . . ?
C42 C41 C44 67.4(18) . . ?
C43 C41 C44 152.4(8) . . ?
C42' C42 C41 67(3) . . ?
C42' C42 C44 128(4) . . ?
C41 C42 C44 61.8(14) . . ?
C42 C42' C41 86(4) . . ?
C43' C43 C41 55.3(8) . . ?
C44' C43' C41 67.2(13) . . ?
C44' C43' C43 130.1(19) . . ?
C41 C43' C43 63.7(11) . . ?
C44' C44 C41 52.6(7) . . ?
C44' C44 C42 94.5(13) . . ?
C41 C44 C42 50.8(9) . . ?
C43' C44' C41 67.2(13) . . ?
C43' C44' C44 134.9(19) . . ?
C41 C44' C44 70.5(10) . . ?
C46 C45 O1 115.3(4) . . ?
C46 C45 H45A 108.4 . . ?
O1 C45 H45A 108.4 . . ?
C46 C45 H45B 108.4 . . ?
O1 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 O3 115.9(9) . . ?
C48 C47 C48' 46.6(11) . . ?
O3 C47 C48' 111.7(11) . . ?
C48' C48 C47 71.7(13) . . ?
C48 C48' C47 61.7(14) . . ?
Cl4 C49 Cl5 112.0(4) . . ?
Cl4 C49 Cl3 110.1(3) . . ?
Cl5 C49 Cl3 110.1(3) . . ?
Cl4 C49 H49 108.2 . . ?
Cl5 C49 H49 108.2 . . ?
Cl3 C49 H49 108.2 . . ?
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
Mo O5 1.650(3) . ?
Mo O2 1.865(2) . ?
Mo O4 1.877(2) . ?
Mo O1 2.371(2) . ?
Mo Cl2 2.3819(12) . ?
Mo Cl1 2.3927(13) . ?
Cl3 C49 1.736(6) . ?
Cl4 C49 1.713(6) . ?
Cl5 C49 1.729(6) . ?
O1 C1 1.409(4) . ?
O1 C45 1.475(4) . ?
O2 C13 1.358(4) . ?
O3 C20 1.380(4) . ?
O3 C47 1.390(6) . ?
O4 C27 1.358(4) . ?
C1 C6 1.376(5) . ?
C1 C2 1.390(5) . ?
C2 C3 1.397(5) . ?
C2 C28 1.518(5) . ?
C3 C4 1.394(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(5) . ?
C4 C29 1.539(5) . ?
C5 C6 1.395(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.517(5) . ?
C7 C8 1.511(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.376(5) . ?
C8 C13 1.405(5) . ?
C9 C10 1.399(6) . ?
C9 H10 0.9300 . ?
C10 C11 1.382(6) . ?
C10 C33 1.528(6) . ?
C11 C12 1.388(5) . ?
C11 H12 0.9300 . ?
C12 C13 1.409(5) . ?
C12 C14 1.509(5) . ?
C14 C15 1.523(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.386(5) . ?
C15 C20 1.388(5) . ?
C16 C17 1.389(6) . ?
C16 H17 0.9300 . ?
C17 C18 1.381(6) . ?
C17 C37 1.534(6) . ?
C18 C19 1.392(5) . ?
C18 H19 0.9300 . ?
C19 C20 1.388(5) . ?
C19 C21 1.526(5) . ?
C21 C22 1.507(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.373(5) . ?
C22 C27 1.404(5) . ?
C23 C24 1.399(5) . ?
C23 H24 0.9300 . ?
C24 C25 1.382(5) . ?
C24 C41 1.545(6) . ?
C25 C26 1.385(5) . ?
C25 H26 0.9300 . ?
C26 C27 1.402(5) . ?
C26 C28 1.507(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C31 1.46(3) . ?
C29 C32 1.497(8) . ?
C29 C30 1.504(7) . ?
C29 C31' 1.62(4) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C31' 0.78(12) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C35 1.512(9) . ?
C33 C36 1.521(9) . ?
C33 C34 1.522(8) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C40 1.494(8) . ?
C37 C38 1.500(7) . ?
C37 C39 1.514(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42' 1.42(2) . ?
C41 C44' 1.477(13) . ?
C41 C43' 1.477(19) . ?
C41 C42 1.54(2) . ?
C41 C43 1.611(12) . ?
C41 C44 1.753(17) . ?
C42 C42' 0.72(7) . ?
C42 C44 1.84(5) . ?
C43 C43' 1.57(3) . ?
C43' C44' 1.15(3) . ?
C44 C44' 1.56(3) . ?
C45 C46 1.423(7) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.362(15) . ?
C47 C48' 1.47(2) . ?
C48 C48' 1.12(3) . ?
C49 H49 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Mo O1 C1 -179.7(6) . . . . ?
O2 Mo O1 C1 -50.4(2) . . . . ?
O4 Mo O1 C1 44.7(2) . . . . ?
Cl2 Mo O1 C1 -139.7(2) . . . . ?
Cl1 Mo O1 C1 131.5(2) . . . . ?
O5 Mo O1 C45 12.5(8) . . . . ?
O2 Mo O1 C45 141.7(3) . . . . ?
O4 Mo O1 C45 -123.1(3) . . . . ?
Cl2 Mo O1 C45 52.5(3) . . . . ?
Cl1 Mo O1 C45 -36.3(3) . . . . ?
O5 Mo O2 C13 87.6(12) . . . . ?
O4 Mo O2 C13 -167.6(12) . . . . ?
O1 Mo O2 C13 -84.4(12) . . . . ?
Cl2 Mo O2 C13 -5.2(12) . . . . ?
Cl1 Mo O2 C13 -77.6(13) . . . . ?
O5 Mo O4 C27 -82.9(7) . . . . ?
O2 Mo O4 C27 173.1(7) . . . . ?
O1 Mo O4 C27 89.9(7) . . . . ?
Cl2 Mo O4 C27 75.7(8) . . . . ?
Cl1 Mo O4 C27 9.2(7) . . . . ?
C45 O1 C1 C6 -100.6(4) . . . . ?
Mo O1 C1 C6 89.8(3) . . . . ?
C45 O1 C1 C2 80.9(4) . . . . ?
Mo O1 C1 C2 -88.8(3) . . . . ?
C6 C1 C2 C3 5.4(5) . . . . ?
O1 C1 C2 C3 -176.1(3) . . . . ?
C6 C1 C2 C28 -174.1(3) . . . . ?
O1 C1 C2 C28 4.4(5) . . . . ?
C1 C2 C3 C4 -1.3(5) . . . . ?
C28 C2 C3 C4 178.2(3) . . . . ?
C2 C3 C4 C5 -2.9(6) . . . . ?
C2 C3 C4 C29 172.4(4) . . . . ?
C3 C4 C5 C6 3.5(6) . . . . ?
C29 C4 C5 C6 -171.8(4) . . . . ?
C2 C1 C6 C5 -5.0(5) . . . . ?
O1 C1 C6 C5 176.6(3) . . . . ?
C2 C1 C6 C7 174.3(3) . . . . ?
O1 C1 C6 C7 -4.2(5) . . . . ?
C4 C5 C6 C1 0.3(5) . . . . ?
C4 C5 C6 C7 -178.9(3) . . . . ?
C1 C6 C7 C8 -105.2(4) . . . . ?
C5 C6 C7 C8 74.0(4) . . . . ?
C6 C7 C8 C9 -111.4(4) . . . . ?
C6 C7 C8 C13 69.0(4) . . . . ?
C13 C8 C9 C10 -0.3(6) . . . . ?
C7 C8 C9 C10 -179.9(4) . . . . ?
C8 C9 C10 C11 1.2(6) . . . . ?
C8 C9 C10 C33 -178.0(4) . . . . ?
C9 C10 C11 C12 -1.6(6) . . . . ?
C33 C10 C11 C12 177.6(4) . . . . ?
C10 C11 C12 C13 1.0(6) . . . . ?
C10 C11 C12 C14 -172.1(4) . . . . ?
Mo O2 C13 C8 76.4(13) . . . . ?
Mo O2 C13 C12 -105.7(12) . . . . ?
C9 C8 C13 O2 177.4(3) . . . . ?
C7 C8 C13 O2 -2.9(5) . . . . ?
C9 C8 C13 C12 -0.4(5) . . . . ?
C7 C8 C13 C12 179.2(3) . . . . ?
C11 C12 C13 O2 -177.8(3) . . . . ?
C14 C12 C13 O2 -4.7(5) . . . . ?
C11 C12 C13 C8 0.0(5) . . . . ?
C14 C12 C13 C8 173.1(3) . . . . ?
C11 C12 C14 C15 107.7(4) . . . . ?
C13 C12 C14 C15 -65.1(5) . . . . ?
C12 C14 C15 C16 -40.7(5) . . . . ?
C12 C14 C15 C20 128.8(4) . . . . ?
C20 C15 C16 C17 -4.6(6) . . . . ?
C14 C15 C16 C17 165.2(4) . . . . ?
C15 C16 C17 C18 -2.9(6) . . . . ?
C15 C16 C17 C37 -179.4(4) . . . . ?
C16 C17 C18 C19 3.5(6) . . . . ?
C37 C17 C18 C19 179.9(4) . . . . ?
C17 C18 C19 C20 3.4(6) . . . . ?
C17 C18 C19 C21 -168.3(4) . . . . ?
C47 O3 C20 C15 83.2(7) . . . . ?
C47 O3 C20 C19 -103.8(6) . . . . ?
C16 C15 C20 O3 -175.5(3) . . . . ?
C14 C15 C20 O3 14.8(5) . . . . ?
C16 C15 C20 C19 11.6(5) . . . . ?
C14 C15 C20 C19 -158.1(3) . . . . ?
C18 C19 C20 O3 175.9(3) . . . . ?
C21 C19 C20 O3 -12.4(5) . . . . ?
C18 C19 C20 C15 -11.1(5) . . . . ?
C21 C19 C20 C15 160.6(3) . . . . ?
C20 C19 C21 C22 -128.3(4) . . . . ?
C18 C19 C21 C22 43.2(5) . . . . ?
C19 C21 C22 C23 -115.8(4) . . . . ?
C19 C21 C22 C27 61.0(5) . . . . ?
C27 C22 C23 C24 -0.2(6) . . . . ?
C21 C22 C23 C24 176.7(4) . . . . ?
C22 C23 C24 C25 -0.9(6) . . . . ?
C22 C23 C24 C41 179.9(4) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
C41 C24 C25 C26 179.6(4) . . . . ?
C24 C25 C26 C27 1.2(6) . . . . ?
C24 C25 C26 C28 -179.9(4) . . . . ?
Mo O4 C27 C26 -79.4(7) . . . . ?
Mo O4 C27 C22 103.3(7) . . . . ?
C25 C26 C27 O4 -179.6(3) . . . . ?
C28 C26 C27 O4 1.5(5) . . . . ?
C25 C26 C27 C22 -2.3(5) . . . . ?
C28 C26 C27 C22 178.8(3) . . . . ?
C23 C22 C27 O4 179.1(3) . . . . ?
C21 C22 C27 O4 2.3(5) . . . . ?
C23 C22 C27 C26 1.8(5) . . . . ?
C21 C22 C27 C26 -175.0(3) . . . . ?
C25 C26 C28 C2 117.9(4) . . . . ?
C27 C26 C28 C2 -63.3(5) . . . . ?
C1 C2 C28 C26 103.7(4) . . . . ?
C3 C2 C28 C26 -75.8(4) . . . . ?
C5 C4 C29 C31 112(7) . . . . ?
C3 C4 C29 C31 -63(7) . . . . ?
C5 C4 C29 C32 -145.5(6) . . . . ?
C3 C4 C29 C32 39.3(7) . . . . ?
C5 C4 C29 C30 -26.7(6) . . . . ?
C3 C4 C29 C30 158.1(5) . . . . ?
C5 C4 C29 C31' 84.1(18) . . . . ?
C3 C4 C29 C31' -91.1(18) . . . . ?
C32 C29 C31 C31' 172(4) . . . . ?
C30 C29 C31 C31' 62(4) . . . . ?
C4 C29 C31 C31' -73(7) . . . . ?
C32 C29 C31' C31 -9(5) . . . . ?
C30 C29 C31' C31 -128(4) . . . . ?
C4 C29 C31' C31 115(5) . . . . ?
C11 C10 C33 C35 -118.5(6) . . . . ?
C9 C10 C33 C35 60.7(7) . . . . ?
C11 C10 C33 C36 120.1(6) . . . . ?
C9 C10 C33 C36 -60.6(7) . . . . ?
C11 C10 C33 C34 -0.2(8) . . . . ?
C9 C10 C33 C34 179.0(5) . . . . ?
C18 C17 C37 C40 -8.3(7) . . . . ?
C16 C17 C37 C40 168.0(6) . . . . ?
C18 C17 C37 C38 -130.7(5) . . . . ?
C16 C17 C37 C38 45.6(6) . . . . ?
C18 C17 C37 C39 109.3(6) . . . . ?
C16 C17 C37 C39 -74.4(6) . . . . ?
C25 C24 C41 C42' -147(4) . . . . ?
C23 C24 C41 C42' 32(4) . . . . ?
C25 C24 C41 C44' 54.5(12) . . . . ?
C23 C24 C41 C44' -126.3(11) . . . . ?
C25 C24 C41 C43' 5.2(16) . . . . ?
C23 C24 C41 C43' -175.6(15) . . . . ?
C25 C24 C41 C42 -177(2) . . . . ?
C23 C24 C41 C42 2(2) . . . . ?
C25 C24 C41 C43 -59.8(8) . . . . ?
C23 C24 C41 C43 119.4(8) . . . . ?
C25 C24 C41 C44 113.0(9) . . . . ?
C23 C24 C41 C44 -67.8(9) . . . . ?
C44' C41 C42 C42' -146(4) . . . . ?
C43' C41 C42 C42' -96(5) . . . . ?
C24 C41 C42 C42' 87(4) . . . . ?
C43 C41 C42 C42' -31(4) . . . . ?
C44 C41 C42 C42' 177(4) . . . . ?
C42' C41 C42 C44 -177(4) . . . . ?
C44' C41 C42 C44 36.5(12) . . . . ?
C43' C41 C42 C44 86(2) . . . . ?
C24 C41 C42 C44 -90.9(13) . . . . ?
C43 C41 C42 C44 151.6(10) . . . . ?
C44 C42 C42' C41 3(5) . . . . ?
C44' C41 C42' C42 46(6) . . . . ?
C43' C41 C42' C42 106(6) . . . . ?
C24 C41 C42' C42 -106(3) . . . . ?
C43 C41 C42' C42 150(4) . . . . ?
C44 C41 C42' C42 -2(4) . . . . ?
C42' C41 C43 C43' -139.7(18) . . . . ?
C44' C41 C43 C43' -6.8(13) . . . . ?
C24 C41 C43 C43' 110.0(11) . . . . ?
C42 C41 C43 C43' -125.7(17) . . . . ?
C44 C41 C43 C43' -54(2) . . . . ?
C42' C41 C43' C44' -118(4) . . . . ?
C24 C41 C43' C44' 93.9(15) . . . . ?
C42 C41 C43' C44' -83(3) . . . . ?
C43 C41 C43' C44' -170.9(17) . . . . ?
C44 C41 C43' C44' -13.5(14) . . . . ?
C42' C41 C43' C43 52(4) . . . . ?
C44' C41 C43' C43 170.9(17) . . . . ?
C24 C41 C43' C43 -95.2(8) . . . . ?
C42 C41 C43' C43 87(3) . . . . ?
C44 C41 C43' C43 157.4(8) . . . . ?
C41 C43 C43' C44' 11.0(19) . . . . ?
C42' C41 C44 C44' 139.9(12) . . . . ?
C43' C41 C44 C44' 11.5(11) . . . . ?
C24 C41 C44 C44' -106.8(7) . . . . ?
C42 C41 C44 C44' 138.7(14) . . . . ?
C43 C41 C44 C44' 58(2) . . . . ?
C42' C41 C44 C42 1(2) . . . . ?
C44' C41 C44 C42 -138.7(14) . . . . ?
C43' C41 C44 C42 -127.2(15) . . . . ?
C24 C41 C44 C42 114.5(12) . . . . ?
C43 C41 C44 C42 -81(2) . . . . ?
C42' C42 C44 C44' -35(6) . . . . ?
C41 C42 C44 C44' -31.7(10) . . . . ?
C42' C42 C44 C41 -3(5) . . . . ?
C43 C43' C44' C41 -10.7(19) . . . . ?
C41 C43' C44' C44 21(2) . . . . ?
C43 C43' C44' C44 11(4) . . . . ?
C42' C41 C44' C43' 102(4) . . . . ?
C24 C41 C44' C43' -105.9(14) . . . . ?
C42 C41 C44' C43' 123.1(19) . . . . ?
C43 C41 C44' C43' 8.3(15) . . . . ?
C44 C41 C44' C43' 164.1(16) . . . . ?
C42' C41 C44' C44 -62(4) . . . . ?
C43' C41 C44' C44 -164.1(16) . . . . ?
C24 C41 C44' C44 90.0(8) . . . . ?
C42 C41 C44' C44 -41.0(15) . . . . ?
C43 C41 C44' C44 -155.8(8) . . . . ?
C41 C44 C44' C43' -21(2) . . . . ?
C42 C44 C44' C43' 10(3) . . . . ?
C42 C44 C44' C41 30.8(10) . . . . ?
C1 O1 C45 C46 67.7(6) . . . . ?
Mo O1 C45 C46 -124.4(5) . . . . ?
C20 O3 C47 C48 145.9(12) . . . . ?
C20 O3 C47 C48' 94.9(17) . . . . ?
O3 C47 C48 C48' -96.1(16) . . . . ?
O3 C47 C48' C48 105.7(14) . . . . ?
