 
data_mr8735o
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C51 H119 Mo8 N5 O27'
_chemical_formula_weight          2002.03
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Mo'  'Mo'  -1.6832   0.6857
 '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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    Pccn
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y+1/2, z'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y-1/2, -z'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y, z-1/2'
 
_cell_length_a                    21.2892(12)
_cell_length_b                    22.0626(10)
_cell_length_c                    16.7364(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      7861.0(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     9964
_cell_measurement_theta_min       2.41
_cell_measurement_theta_max       27.4
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.09
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     1.692
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              4048
_exptl_absorpt_coefficient_mu     1.304
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.8916
_exptl_absorpt_correction_T_max   0.9142
_exptl_absorpt_process_details    SADABS
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker Apex II Quasar'
_diffrn_measurement_method        'ω & π scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         none
_diffrn_reflns_number             32104
_diffrn_reflns_av_R_equivalents   0.0360
_diffrn_reflns_av_sigmaI/netI     0.0335
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        25
_diffrn_reflns_limit_k_min        -24
_diffrn_reflns_limit_k_max        27
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.80
_diffrn_reflns_theta_max          26.00
_reflns_number_total              7648
_reflns_number_gt                 6341
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        Apex2
_computing_cell_refinement        Apex2
_computing_data_reduction         Apex2
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0237P)²+13.1538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.000153(17)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          7648
_refine_ls_number_parameters      418
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0391
_refine_ls_R_factor_gt            0.0276
_refine_ls_wR_factor_ref          0.0688
_refine_ls_wR_factor_gt           0.0610
_refine_ls_goodness_of_fit_ref    1.059
_refine_ls_restrained_S_all       1.059
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
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 0.051559(12) 0.543324(12) 0.435441(16) 0.01503(7) Uani 1 1 d . . .
Mo2 Mo -0.060906(13) 0.630165(13) 0.572950(16) 0.01729(8) Uani 1 1 d . . .
Mo3 Mo -0.064843(13) 0.433680(14) 0.339296(17) 0.02102(8) Uani 1 1 d . . .
Mo4 Mo -0.124552(13) 0.563539(13) 0.410903(16) 0.01719(8) Uani 1 1 d . . .
O1 O -0.02239(10) 0.58779(10) 0.65902(13) 0.0213(5) Uani 1 1 d . . .
O2 O -0.07652(10) 0.62620(9) 0.46094(12) 0.0175(5) Uani 1 1 d . . .
O3 O -0.13399(10) 0.63942(10) 0.61193(13) 0.0236(5) Uani 1 1 d . . .
O4 O -0.02710(11) 0.69994(11) 0.57884(14) 0.0269(6) Uani 1 1 d . . .
O5 O -0.10020(11) 0.36463(11) 0.33347(15) 0.0320(6) Uani 1 1 d . . .
O6 O -0.13002(10) 0.47840(10) 0.39187(13) 0.0208(5) Uani 1 1 d . . .
O7 O -0.19730(10) 0.57478(10) 0.44997(14) 0.0256(5) Uani 1 1 d . . .
O8 O -0.12846(11) 0.59304(11) 0.31702(14) 0.0275(6) Uani 1 1 d . . .
O9 O -0.06912(11) 0.46169(12) 0.24486(14) 0.0323(6) Uani 1 1 d . . .
O10 O -0.02091(10) 0.52730(10) 0.38606(13) 0.0197(5) Uani 1 1 d . . .
O11 O 0.03642(10) 0.58566(10) 0.52425(13) 0.0201(5) Uani 1 1 d . . .
O12 O 0.09921(10) 0.58503(10) 0.37384(14) 0.0247(5) Uani 1 1 d . . .
O13 O 0.08967(10) 0.47435(10) 0.46078(12) 0.0180(5) Uani 1 1 d . . .
N1 N 0.99062(13) 0.26162(13) 0.16900(16) 0.0228(6) Uani 1 1 d . . .
N2 N 0.76508(12) 0.48756(13) 0.15430(16) 0.0223(6) Uani 1 1 d . . .
N3 N 0.2550(14) 0.2562(14) 0.0182(10) 0.053(7) Uiso 0.25 1 d PD . .
N3' N 0.2403(7) 0.2726(6) 0.0210(7) 0.009(2) Uiso 0.25 1 d PD . .
C1 C 0.95836(16) 0.22934(16) 0.0997(2) 0.0278(8) Uani 1 1 d . . .
H1A H 0.9834 0.2362 0.0507 0.033 Uiso 1 1 calc R . .
H1B H 0.9586 0.1852 0.1106 0.033 Uiso 1 1 calc R . .
C2 C 0.89114(18) 0.2489(2) 0.0834(3) 0.0428(11) Uani 1 1 d . . .
H2A H 0.8654 0.2428 0.1320 0.051 Uiso 1 1 calc R . .
H2B H 0.8902 0.2925 0.0696 0.051 Uiso 1 1 calc R . .
C3 C 0.86377(19) 0.21217(18) 0.0150(2) 0.0417(10) Uani 1 1 d . . .
H3A H 0.8205 0.2252 0.0050 0.063 Uiso 1 1 calc R . .
H3B H 0.8641 0.1691 0.0291 0.063 Uiso 1 1 calc R . .
H3C H 0.8891 0.2185 -0.0332 0.063 Uiso 1 1 calc R . .
C4 C 0.98677(17) 0.33022(15) 0.1594(2) 0.0254(8) Uani 1 1 d . . .
H4A H 0.9422 0.3425 0.1634 0.030 Uiso 1 1 calc R . .
H4B H 1.0095 0.3493 0.2044 0.030 Uiso 1 1 calc R . .
C5 C 1.0133(2) 0.35498(18) 0.0819(2) 0.0388(10) Uani 1 1 d . . .
H5A H 0.9944 0.3332 0.0360 0.047 Uiso 1 1 calc R . .
H5B H 1.0593 0.3486 0.0804 0.047 Uiso 1 1 calc R . .
C6 C 0.9989(2) 0.42223(18) 0.0752(3) 0.0455(11) Uani 1 1 d . . .
H6A H 1.0158 0.4379 0.0249 0.068 Uiso 1 1 calc R . .
H6B H 1.0183 0.4438 0.1201 0.068 Uiso 1 1 calc R . .
H6C H 0.9533 0.4284 0.0765 0.068 Uiso 1 1 calc R . .
C7 C 1.05917(15) 0.24102(16) 0.1691(2) 0.0262(8) Uani 1 1 d . . .
H7A H 1.0602 0.1962 0.1684 0.031 Uiso 1 1 calc R . .
H7B H 1.0794 0.2555 0.1194 0.031 Uiso 1 1 calc R . .
C8 C 1.09721(16) 0.26317(18) 0.2398(2) 0.0323(9) Uani 1 1 d . . .
H8A H 1.0784 0.2476 0.2899 0.039 Uiso 1 1 calc R . .
H8B H 1.0960 0.3080 0.2417 0.039 Uiso 1 1 calc R . .
C9 C 1.16506(17) 0.2420(2) 0.2338(3) 0.0450(11) Uani 1 1 d . . .
H9A H 1.1887 0.2567 0.2802 0.068 Uiso 1 1 calc R . .
H9B H 1.1839 0.2581 0.1848 0.068 Uiso 1 1 calc R . .
H9C H 1.1663 0.1976 0.2325 0.068 Uiso 1 1 calc R . .
C10 C 0.95884(16) 0.24633(17) 0.2478(2) 0.0266(8) Uani 1 1 d . . .
H10A H 0.9795 0.2698 0.2908 0.032 Uiso 1 1 calc R . .
H10B H 0.9146 0.2599 0.2450 0.032 Uiso 1 1 calc R . .
C11 C 0.9597(2) 0.17988(17) 0.2710(2) 0.0381(10) Uani 1 1 d . . .
H11A H 1.0034 0.1645 0.2699 0.046 Uiso 1 1 calc R . .
H11B H 0.9347 0.1561 0.2322 0.046 Uiso 1 1 calc R . .
C12 C 0.9323(2) 0.1723(2) 0.3545(3) 0.0517(12) Uani 1 1 d . . .
H12A H 0.9332 0.1294 0.3695 0.077 Uiso 1 1 calc R . .
H12B H 0.8888 0.1869 0.3550 0.077 Uiso 1 1 calc R . .
H12C H 0.9573 0.1958 0.3927 0.077 Uiso 1 1 calc R . .
C13 C 0.78221(16) 0.43381(15) 0.2063(2) 0.0245(8) Uani 1 1 d . . .
H13A H 0.8182 0.4126 0.1814 0.029 Uiso 1 1 calc R . .
H13B H 0.7964 0.4493 0.2588 0.029 Uiso 1 1 calc R . .
C14 C 0.73053(17) 0.38795(17) 0.2205(2) 0.0338(9) Uani 1 1 d . . .
H14A H 0.7104 0.3774 0.1690 0.041 Uiso 1 1 calc R . .
H14B H 0.6981 0.4057 0.2558 0.041 Uiso 1 1 calc R . .
C15 C 0.75719(18) 0.33121(16) 0.2588(2) 0.0362(9) Uani 1 1 d . . .
H15A H 0.7233 0.3019 0.2677 0.054 Uiso 1 1 calc R . .
H15B H 0.7766 0.3417 0.3100 0.054 Uiso 1 1 calc R . .
H15C H 0.7888 0.3134 0.2234 0.054 Uiso 1 1 calc R . .
C16 C 0.82217(16) 0.52886(16) 0.1528(2) 0.0275(8) Uani 1 1 d . . .
H16A H 0.8323 0.5402 0.2086 0.033 Uiso 1 1 calc R . .
H16B H 0.8582 0.5053 0.1318 0.033 Uiso 1 1 calc R . .
C17 C 0.81655(19) 0.58622(19) 0.1044(2) 0.0406(10) Uani 1 1 d . . .
H17A H 0.7826 0.6120 0.1263 0.049 Uiso 1 1 calc R . .
H17B H 0.8062 0.5763 0.0483 0.049 Uiso 1 1 calc R . .
C18 C 0.8789(2) 0.6197(2) 0.1084(3) 0.0458(11) Uani 1 1 d . . .
H18A H 0.8760 0.6573 0.0774 0.069 Uiso 1 1 calc R . .
H18B H 0.9122 0.5941 0.0862 0.069 Uiso 1 1 calc R . .
H18C H 0.8887 0.6294 0.1642 0.069 Uiso 1 1 calc R . .
C19 C 0.74745(17) 0.46698(16) 0.0707(2) 0.0273(8) Uani 1 1 d . . .
H19A H 0.7097 0.4409 0.0746 0.033 Uiso 1 1 calc R . .
H19B H 0.7357 0.5032 0.0391 0.033 Uiso 1 1 calc R . .
C20 C 0.7975(2) 0.4327(2) 0.0256(3) 0.0514(12) Uiso 1 1 d . . .
H20A H 0.8346 0.4591 0.0178 0.062 Uiso 1 1 calc R . .
H20B H 0.8108 0.3970 0.0571 0.062 Uiso 1 1 calc R . .
C21 C 0.7729(2) 0.4123(2) -0.0545(3) 0.0502(12) Uiso 1 1 d . . .
H21A H 0.8058 0.3898 -0.0828 0.075 Uiso 1 1 calc R . .
H21B H 0.7607 0.4478 -0.0861 0.075 Uiso 1 1 calc R . .
H21C H 0.7363 0.3860 -0.0466 0.075 Uiso 1 1 calc R . .
C22 C 0.70787(16) 0.52020(17) 0.1871(2) 0.0273(8) Uani 1 1 d . . .
H22A H 0.6724 0.4912 0.1891 0.033 Uiso 1 1 calc R . .
H22B H 0.6962 0.5529 0.1494 0.033 Uiso 1 1 calc R . .
C23 C 0.71610(19) 0.54777(19) 0.2696(2) 0.0385(10) Uani 1 1 d . . .
H23A H 0.7384 0.5189 0.3049 0.046 Uiso 1 1 calc R . .
H23B H 0.7415 0.5853 0.2658 0.046 Uiso 1 1 calc R . .
C24 C 0.6524(2) 0.5622(2) 0.3042(3) 0.0605(13) Uiso 1 1 d . . .
H24A H 0.6250 0.5778 0.2619 0.091 Uiso 1 1 calc R . .
H24B H 0.6569 0.5928 0.3462 0.091 Uiso 1 1 calc R . .
H24C H 0.6340 0.5253 0.3269 0.091 Uiso 1 1 calc R . .
O14 O 0.3360(3) 0.1762(3) 0.0667(4) 0.0515(16) Uani 0.50 1 d P . .
C30 C 0.2795(4) 0.1871(4) 0.0605(5) 0.039(2) Uani 0.50 1 d P . .
C31 C 0.1885(5) 0.2414(5) 0.0114(6) 0.041(3) Uani 0.50 1 d PD . .
C32 C 0.2979(6) 0.2743(6) -0.0238(7) 0.052(3) Uani 0.50 1 d PD . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Mo1 O12 1.714(2) . ?
Mo1 O13 1.776(2) . ?
Mo1 O11 1.785(2) . ?
Mo1 O10 1.786(2) . ?
Mo2 O3 1.700(2) . ?
Mo2 O4 1.702(2) . ?
Mo2 O1 1.903(2) . ?
Mo2 O2 1.906(2) . ?
Mo2 O11 2.433(2) . ?
Mo2 O13 2.452(2) 5_566 ?
Mo3 O9 1.699(2) . ?
Mo3 O5 1.702(2) . ?
Mo3 O6 1.917(2) . ?
Mo3 O1 1.917(2) 5_566 ?
Mo3 O10 2.399(2) . ?
Mo3 O11 2.401(2) 5_566 ?
Mo4 O7 1.699(2) . ?
Mo4 O8 1.703(2) . ?
Mo4 O6 1.909(2) . ?
Mo4 O2 1.913(2) . ?
Mo4 O10 2.383(2) . ?
Mo4 O13 2.421(2) 5_566 ?
O1 Mo3 1.917(2) 5_566 ?
O11 Mo3 2.401(2) 5_566 ?
O13 Mo4 2.421(2) 5_566 ?
O13 Mo2 2.452(2) 5_566 ?
N1 C10 1.520(4) . ?
N1 C4 1.524(4) . ?
N1 C1 1.525(4) . ?
N1 C7 1.528(4) . ?
N2 C13 1.516(4) . ?
N2 C22 1.518(4) . ?
N2 C19 1.518(4) . ?
N2 C16 1.519(4) . ?
N3 N3 0.35(7) 2 ?
N3 N3' 0.64(3) 2 ?
N3 C31 1.21(3) 2 ?
N3 C32 1.22(3) . ?
N3 C31 1.46(3) . ?
N3 C32 1.49(3) 2 ?
N3 C30 1.61(2) 2 ?
N3 C30 1.76(3) . ?
N3' N3 0.64(3) 2 ?
N3' N3' 1.08(3) 2 ?
N3' C30 1.185(15) 2 ?
N3' C31 1.309(17) . ?
N3' C32 1.438(19) . ?
N3' C32 1.515(16) 2 ?
N3' C31 1.554(18) 2 ?
C1 C2 1.519(5) . ?
C2 C3 1.518(5) . ?
C4 C5 1.517(5) . ?
C5 C6 1.519(5) . ?
C7 C8 1.514(5) . ?
C8 C9 1.521(5) . ?
C10 C11 1.516(5) . ?
C11 C12 1.524(6) . ?
C13 C14 1.513(5) . ?
C14 C15 1.517(5) . ?
C16 C17 1.507(5) . ?
C17 C18 1.522(5) . ?
C19 C20 1.508(6) . ?
C20 C21 1.508(6) . ?
C22 C23 1.519(5) . ?
C23 C24 1.508(6) . ?
O14 C30 1.232(10) . ?
C30 N3' 1.185(15) 2 ?
C30 N3 1.61(2) 2 ?
C30 C31 1.904(14) 2 ?
C31 C32 0.742(12) 2 ?
C31 N3 1.21(3) 2 ?
C31 N3' 1.554(18) 2 ?
C31 C30 1.904(14) 2 ?
C32 C31 0.742(12) 2 ?
C32 N3 1.49(3) 2 ?
C32 N3' 1.515(16) 2 ?
 
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
O12 Mo1 O13 109.46(10) . . ?
O12 Mo1 O11 109.08(11) . . ?
O13 Mo1 O11 109.40(10) . . ?
O12 Mo1 O10 109.83(11) . . ?
O13 Mo1 O10 109.61(10) . . ?
O11 Mo1 O10 109.45(10) . . ?
O3 Mo2 O4 104.85(11) . . ?
O3 Mo2 O1 99.38(10) . . ?
O4 Mo2 O1 102.60(11) . . ?
O3 Mo2 O2 102.91(10) . . ?
O4 Mo2 O2 99.92(10) . . ?
O1 Mo2 O2 142.86(9) . . ?
O3 Mo2 O11 163.06(9) . . ?
O4 Mo2 O11 91.39(9) . . ?
O1 Mo2 O11 71.85(8) . . ?
O2 Mo2 O11 78.49(8) . . ?
O3 Mo2 O13 88.44(9) . 5_566 ?
O4 Mo2 O13 165.82(9) . 5_566 ?
O1 Mo2 O13 79.62(8) . 5_566 ?
O2 Mo2 O13 71.75(8) . 5_566 ?
O11 Mo2 O13 75.88(7) . 5_566 ?
O9 Mo3 O5 104.39(12) . . ?
O9 Mo3 O6 101.59(10) . . ?
O5 Mo3 O6 99.61(11) . . ?
O9 Mo3 O1 98.94(10) . 5_566 ?
O5 Mo3 O1 102.01(11) . 5_566 ?
O6 Mo3 O1 145.28(9) . 5_566 ?
O9 Mo3 O10 90.64(10) . . ?
O5 Mo3 O10 164.12(10) . . ?
O6 Mo3 O10 71.89(8) . . ?
O1 Mo3 O10 80.23(8) 5_566 . ?
O9 Mo3 O11 164.32(10) . 5_566 ?
O5 Mo3 O11 90.39(10) . 5_566 ?
O6 Mo3 O11 80.64(8) . 5_566 ?
O1 Mo3 O11 72.42(8) 5_566 5_566 ?
O10 Mo3 O11 75.19(7) . 5_566 ?
O7 Mo4 O8 104.75(11) . . ?
O7 Mo4 O6 98.75(10) . . ?
O8 Mo4 O6 102.66(11) . . ?
O7 Mo4 O2 102.32(10) . . ?
O8 Mo4 O2 98.85(10) . . ?
O6 Mo4 O2 144.78(9) . . ?
O7 Mo4 O10 163.70(9) . . ?
O8 Mo4 O10 90.72(10) . . ?
O6 Mo4 O10 72.38(8) . . ?
O2 Mo4 O10 79.86(8) . . ?
O7 Mo4 O13 89.35(9) . 5_566 ?
O8 Mo4 O13 164.89(9) . 5_566 ?
O6 Mo4 O13 80.04(8) . 5_566 ?
O2 Mo4 O13 72.37(8) . 5_566 ?
O10 Mo4 O13 75.82(7) . 5_566 ?
Mo2 O1 Mo3 123.36(12) . 5_566 ?
Mo2 O2 Mo4 123.86(11) . . ?
Mo4 O6 Mo3 122.62(11) . . ?
Mo1 O10 Mo4 130.75(11) . . ?
Mo1 O10 Mo3 131.18(11) . . ?
Mo4 O10 Mo3 89.13(7) . . ?
Mo1 O11 Mo3 130.82(11) . 5_566 ?
Mo1 O11 Mo2 130.08(11) . . ?
Mo3 O11 Mo2 88.15(7) 5_566 . ?
Mo1 O13 Mo4 130.37(11) . 5_566 ?
Mo1 O13 Mo2 129.56(11) . 5_566 ?
Mo4 O13 Mo2 87.49(7) 5_566 5_566 ?
C10 N1 C4 106.7(2) . . ?
C10 N1 C1 110.9(3) . . ?
C4 N1 C1 111.1(3) . . ?
C10 N1 C7 111.0(3) . . ?
C4 N1 C7 110.3(3) . . ?
C1 N1 C7 107.0(2) . . ?
C13 N2 C22 110.9(3) . . ?
C13 N2 C19 110.8(3) . . ?
C22 N2 C19 106.1(2) . . ?
C13 N2 C16 106.6(2) . . ?
C22 N2 C16 111.3(3) . . ?
C19 N2 C16 111.2(3) . . ?
N3 N3 N3' 47(6) 2 2 ?
N3 N3 C31 130(9) 2 2 ?
N3' N3 C31 84(3) 2 2 ?
N3 N3 C32 136(5) 2 . ?
N3' N3 C32 104(3) 2 . ?
C31 N3 C32 35.6(11) 2 . ?
N3 N3 C31 39(7) 2 . ?
N3' N3 C31 86(3) 2 . ?
C31 N3 C31 166(2) 2 . ?
C32 N3 C31 139.1(17) . . ?
N3 N3 C32 35(4) 2 2 ?
N3' N3 C32 73(3) 2 2 ?
C31 N3 C32 136.8(18) 2 2 ?
C32 N3 C32 116.3(17) . 2 ?
C31 N3 C32 29.2(8) . 2 ?
N3 N3 C30 109(8) 2 2 ?
N3' N3 C30 143(3) 2 2 ?
C31 N3 C30 117(2) 2 2 ?
C32 N3 C30 110(2) . 2 ?
C31 N3 C30 76.4(13) . 2 ?
C32 N3 C30 102.3(16) 2 2 ?
N3 N3 C30 60(7) 2 . ?
N3' N3 C30 22(2) 2 . ?
C31 N3 C30 77.4(14) 2 . ?
C32 N3 C30 107.1(18) . . ?
C31 N3 C30 97.2(19) . . ?
C32 N3 C30 91.3(18) 2 . ?
C30 N3 C30 129.1(12) 2 . ?
N3 N3' N3' 14(3) 2 2 ?
N3 N3' C30 147(3) 2 2 ?
N3' N3' C30 146.0(7) 2 2 ?
N3 N3' C31 67(3) 2 . ?
N3' N3' C31 80.6(14) 2 . ?
C30 N3' C31 99.4(12) 2 . ?
N3 N3' C32 82(3) 2 . ?
N3' N3' C32 72.5(13) 2 . ?
C30 N3' C32 125.0(12) 2 . ?
C31 N3' C32 131.9(12) . . ?
N3 N3' C32 51(2) 2 2 ?
N3' N3' C32 64.8(11) 2 2 ?
C30 N3' C32 126.7(13) 2 2 ?
C31 N3' C32 29.3(6) . 2 ?
C32 N3' C32 102.6(12) . 2 ?
N3 N3' C31 69(3) 2 2 ?
N3' N3' C31 56.2(13) 2 2 ?
C30 N3' C31 123.6(11) 2 2 ?
C31 N3' C31 134.7(11) . 2 ?
C32 N3' C31 28.4(5) . 2 ?
C32 N3' C31 109.7(11) 2 2 ?
C2 C1 N1 115.4(3) . . ?
C3 C2 C1 110.2(3) . . ?
C5 C4 N1 115.3(3) . . ?
C4 C5 C6 109.8(3) . . ?
C8 C7 N1 114.6(3) . . ?
C7 C8 C9 110.9(3) . . ?
C11 C10 N1 115.5(3) . . ?
C10 C11 C12 109.6(3) . . ?
C14 C13 N2 116.0(3) . . ?
C13 C14 C15 110.2(3) . . ?
C17 C16 N2 116.7(3) . . ?
C16 C17 C18 108.4(3) . . ?
C20 C19 N2 115.9(3) . . ?
C21 C20 C19 110.5(4) . . ?
N2 C22 C23 115.2(3) . . ?
C24 C23 C22 109.2(3) . . ?
N3' C30 O14 122.8(10) 2 . ?
N3' C30 N3 9.0(11) 2 2 ?
O14 C30 N3 129.2(14) . 2 ?
N3' C30 N3 11.6(10) 2 . ?
O14 C30 N3 119.5(12) . . ?
N3 C30 N3 11(2) 2 . ?
N3' C30 C31 42.7(8) 2 2 ?
O14 C30 C31 81.3(6) . 2 ?
N3 C30 C31 48.0(13) 2 2 ?
N3 C30 C31 38.3(11) . 2 ?
C32 C31 N3 73.1(18) 2 2 ?
C32 C31 N3' 90.9(18) 2 . ?
N3 C31 N3' 29.3(18) 2 . ?
C32 C31 N3 77.8(18) 2 . ?
N3 C31 N3 10(3) 2 . ?
N3' C31 N3 19.1(10) . . ?
C32 C31 N3' 67.1(17) 2 2 ?
N3 C31 N3' 14.0(16) 2 2 ?
N3' C31 N3' 43.2(11) . 2 ?
N3 C31 N3' 24.4(12) . 2 ?
C32 C31 C30 126.2(18) 2 2 ?
N3 C31 C30 64.4(15) 2 2 ?
N3' C31 C30 37.9(7) . 2 ?
N3 C31 C30 55.5(11) . 2 ?
N3' C31 C30 76.8(7) 2 2 ?
C31 C32 N3 71.3(18) 2 . ?
C31 C32 N3' 84.5(17) 2 . ?
N3 C32 N3' 18.6(12) . . ?
C31 C32 N3 73.0(17) 2 2 ?
N3 C32 N3 9(2) . 2 ?
N3' C32 N3 25.3(13) . 2 ?
C31 C32 N3' 59.7(15) 2 2 ?
N3 C32 N3' 24.3(16) . 2 ?
N3' C32 N3' 42.7(11) . 2 ?
N3 C32 N3' 18.4(8) 2 2 ?
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              26.00
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    1.04 
_refine_diff_density_min   -0.55 
_refine_diff_density_rms    0.11
