 
data_mr719
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C35 H83 Mn Mo6 N6 O25'
_chemical_formula_weight          1618.65
 
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'
 'Mn'  'Mn'   0.3368   0.7283
 '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            Monoclinic
_symmetry_space_group_name_H-M    C2/m
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    15.0770(13)
_cell_length_b                    23.102(2)
_cell_length_c                    15.0791(14)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.336(5)
_cell_angle_gamma                 90.00
_cell_volume                      5247.9(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     7194
_cell_measurement_theta_min       2.22
_cell_measurement_theta_max       28.5
 
_exptl_crystal_description        block
_exptl_crystal_colour             orange
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     2.049
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3248
_exptl_absorpt_coefficient_mu     1.708
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.7374
_exptl_absorpt_correction_T_max   0.8898
_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        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         none
_diffrn_reflns_number             19081
_diffrn_reflns_av_R_equivalents   0.0293
_diffrn_reflns_av_sigmaI/netI     0.0288
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -28
_diffrn_reflns_limit_k_max        28
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          1.61
_diffrn_reflns_theta_max          26.00
_reflns_number_total              5245
_reflns_number_gt                 4121
_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)+(0.0722P)²+47.0481P] 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        0.000110(16)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5245
_refine_ls_number_parameters      333
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0605
_refine_ls_R_factor_gt            0.0456
_refine_ls_wR_factor_ref          0.1447
_refine_ls_wR_factor_gt           0.1279
_refine_ls_goodness_of_fit_ref    1.032
_refine_ls_restrained_S_all       1.032
_refine_ls_shift/su_max           0.005
_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 0.090488(17) 0.072120(12) 0.835404(17) 0.05093(7) Uani 1 1 d . . .
Mo2 Mo 0.0000 0.145947(14) 1.0000 0.06135(13) Uani 1 2 d S . .
Mo3 Mo 0.322687(14) 0.072338(9) 0.419328(15) 0.03364(6) Uani 1 1 d . . .
Mo4 Mo 0.5000 0.144998(12) 0.5000 0.03379(8) Uani 1 2 d S . .
Mn1 Mn 0.0000 0.0000 1.0000 0.02269(16) Uani 1 4 d S . .
Mn2 Mn 0.5000 0.0000 0.5000 0.02291(16) Uani 1 4 d S . .
O1 O 0.11258(15) 0.0000 0.94520(15) 0.0320(6) Uani 1 2 d S . .
O2 O -0.03802(11) 0.06301(7) 0.91480(12) 0.0365(5) Uani 1 1 d . . .
O3 O 0.04995(18) 0.19022(10) 1.0765(2) 0.0855(9) Uani 1 1 d . . .
O4 O 0.10230(13) 0.12082(8) 0.93909(15) 0.0568(6) Uani 1 1 d . . .
O5 O 0.19961(15) 0.06956(12) 0.81103(16) 0.0758(8) Uani 1 1 d . . .
O6 O 0.04750(17) 0.0000 0.78914(16) 0.0476(8) Uani 1 2 d S . .
O7 O 0.04267(16) 0.11651(11) 0.75838(16) 0.0816(8) Uani 1 1 d . . .
O8 O 0.42632(15) 0.0000 0.38649(15) 0.0313(6) Uani 1 2 d S . .
O9 O 0.28280(15) 0.0000 0.46474(17) 0.0358(6) Uani 1 2 d S . .
O10 O 0.27835(13) 0.07121(8) 0.31376(14) 0.0459(6) Uani 1 1 d . . .
O11 O 0.25661(12) 0.11732(8) 0.47667(14) 0.0482(6) Uani 1 1 d . . .
O12 O 0.42383(11) 0.12028(7) 0.40200(11) 0.0351(4) Uani 1 1 d . . .
O13 O 0.43191(13) 0.18930(8) 0.55577(13) 0.0454(5) Uani 1 1 d . . .
O14 O 0.42235(11) 0.06179(7) 0.54230(11) 0.0319(4) Uani 1 1 d . . .
N1 N 0.2602(2) 0.0000 1.1482(2) 0.0484(10) Uani 1 2 d S . .
H1A H 0.2871 0.0347 1.1398 0.073 Uiso 0.33 1 calc PR . .
H1B H 0.2940 -0.0288 1.1258 0.073 Uiso 0.33 1 calc PR . .
H1C H 0.2539 -0.0060 1.2072 0.073 Uiso 0.33 1 calc PR . .
N2 N 0.3878(2) 0.0000 0.7676(2) 0.0555(11) Uani 1 2 d S . .
H2A H 0.3339 0.0178 0.7655 0.083 Uiso 0.33 1 calc PR . .
H2B H 0.4254 0.0194 0.8059 0.083 Uiso 0.33 1 calc PR . .
H2C H 0.3816 -0.0371 0.7866 0.083 Uiso 0.33 1 calc PR . .
N3 N 0.23039(17) 0.24393(11) 0.71706(18) 0.0547(7) Uani 1 1 d . . .
N6 N 0.2493(3) 0.1874(2) 0.0225(3) 0.0447(11) Uiso 0.50 1 d P . .
C1 C 0.1915(2) 0.0000 1.0024(2) 0.0375(10) Uani 1 2 d S . .
H1D H 0.2274 0.0346 0.9893 0.045 Uiso 0.50 1 calc PR . .
H1E H 0.2274 -0.0346 0.9893 0.045 Uiso 0.50 1 calc PR . .
C2 C -0.12356(17) 0.05555(12) 0.87030(19) 0.0415(7) Uani 1 1 d . . .
H2D H -0.1159 0.0545 0.8054 0.050 Uiso 1 1 calc R . .
H2E H -0.1613 0.0894 0.8832 0.050 Uiso 1 1 calc R . .
C3 C 0.1713(2) 0.0000 1.1017(2) 0.0370(9) Uani 1 2 d S . .
C4 C 0.39178(17) 0.05511(12) 0.63137(17) 0.0394(7) Uani 1 1 d . . .
H4A H 0.3261 0.0552 0.6288 0.047 Uiso 1 1 calc R . .
H4B H 0.4118 0.0889 0.6671 0.047 Uiso 1 1 calc R . .
C5 C 0.4739(2) 0.0000 0.3065(2) 0.0372(9) Uani 1 2 d S . .
H5A H 0.4563 0.0346 0.2712 0.045 Uiso 0.50 1 calc PR . .
H5B H 0.4563 -0.0346 0.2712 0.045 Uiso 0.50 1 calc PR . .
C6 C 0.4242(3) 0.0000 0.6784(2) 0.0404(10) Uani 1 2 d S . .
C7 C 0.1949(2) 0.24943(14) 0.6214(2) 0.0541(9) Uani 1 1 d . . .
H7A H 0.1697 0.2887 0.6129 0.065 Uiso 1 1 calc R . .
H7B H 0.2452 0.2457 0.5817 0.065 Uiso 1 1 calc R . .
C8 C 0.1253(2) 0.20605(14) 0.5934(2) 0.0612(10) Uani 1 1 d . . .
H8A H 0.1515 0.1672 0.5935 0.092 Uiso 1 1 calc R . .
H8B H 0.1020 0.2154 0.5334 0.092 Uiso 1 1 calc R . .
H8C H 0.0769 0.2072 0.6348 0.092 Uiso 1 1 calc R . .
C9 C 0.2834(2) 0.18854(13) 0.7212(2) 0.0643(10) Uani 1 1 d . . .
H9A H 0.3257 0.1888 0.6727 0.077 Uiso 1 1 calc R . .
H9B H 0.2424 0.1556 0.7106 0.077 Uiso 1 1 calc R . .
C10 C 0.3348(3) 0.17890(17) 0.8086(3) 0.0882(14) Uani 1 1 d . . .
H10A H 0.3769 0.2107 0.8190 0.132 Uiso 1 1 calc R . .
H10B H 0.3673 0.1422 0.8062 0.132 Uiso 1 1 calc R . .
H10C H 0.2934 0.1775 0.8570 0.132 Uiso 1 1 calc R . .
C11 C 0.2884(2) 0.29599(13) 0.7419(2) 0.0595(10) Uani 1 1 d . . .
H11A H 0.2509 0.3312 0.7392 0.071 Uiso 1 1 calc R . .
H11B H 0.3108 0.2913 0.8041 0.071 Uiso 1 1 calc R . .
C12 C 0.3660(2) 0.30538(16) 0.6849(3) 0.0692(11) Uani 1 1 d . . .
H12A H 0.4039 0.2709 0.6869 0.104 Uiso 1 1 calc R . .
H12B H 0.4002 0.3389 0.7069 0.104 Uiso 1 1 calc R . .
H12C H 0.3448 0.3125 0.6236 0.104 Uiso 1 1 calc R . .
C13 C 0.1572(3) 0.23968(15) 0.7817(2) 0.0654(11) Uani 1 1 d . . .
H13A H 0.1842 0.2393 0.8426 0.078 Uiso 1 1 calc R . .
H13B H 0.1262 0.2023 0.7722 0.078 Uiso 1 1 calc R . .
C14 C 0.0888(3) 0.28812(17) 0.7752(3) 0.0820(13) Uani 1 1 d . . .
H14A H 0.1185 0.3255 0.7845 0.123 Uiso 1 1 calc R . .
H14B H 0.0449 0.2825 0.8206 0.123 Uiso 1 1 calc R . .
H14C H 0.0589 0.2875 0.7163 0.123 Uiso 1 1 calc R . .
N4 N 0.0000 0.0000 0.5000 0.0821(19) Uiso 1 4 d S . .
C15 C 0.1395(6) 0.0000 0.6020(6) 0.063(2) Uiso 0.60 2 d SP . .
C16 C 0.1353(6) 0.0278(4) 0.5997(6) 0.046(2) Uiso 0.30 1 d P . .
C17 C 0.0418(12) 0.0256(8) 0.5848(12) 0.068(5) Uiso 0.20 1 d P . .
C17' C 0.0930(18) 0.0000 0.5047(18) 0.067(6) Uiso 0.20 2 d SP . .
C18 C -0.0262(17) 0.0806(10) 0.5388(16) 0.096(7) Uiso 0.20 1 d P . .
C19 C -0.0578(13) 0.0313(9) 0.5764(13) 0.078(5) Uiso 0.20 1 d P . .
N5 N 0.5000 0.1069(6) 0.0000 0.091(4) Uiso 0.40 2 d SP . 1
O15 O 0.3637(3) 0.0894(2) 0.0776(3) 0.0667(12) Uiso 0.50 1 d P A 1
C20 C 0.4290(9) 0.0771(6) 0.0436(9) 0.091(4) Uiso 0.35 1 d P A 1
C21 C 0.5000 0.1707(4) 0.0000 0.060(2) Uiso 0.50 2 d SP B 1
 
 
_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 O7 1.689(2) . ?
Mo1 O5 1.701(2) . ?
Mo1 O6 1.9094(13) . ?
Mo1 O4 1.929(2) . ?
Mo1 O2 2.3283(18) . ?
Mo1 O1 2.3629(16) . ?
Mo2 O3 1.695(3) . ?
Mo2 O3 1.695(3) 2_557 ?
Mo2 O4 1.917(2) 2_557 ?
Mo2 O4 1.917(2) . ?
Mo2 O2 2.3645(17) . ?
Mo2 O2 2.3645(17) 2_557 ?
Mo3 O11 1.7002(19) . ?
Mo3 O10 1.701(2) . ?
Mo3 O12 1.9112(17) . ?
Mo3 O9 1.9123(12) . ?
Mo3 O14 2.3513(16) . ?
Mo3 O8 2.3543(16) . ?
Mo4 O13 1.6968(19) . ?
Mo4 O13 1.6968(19) 2_656 ?
Mo4 O12 1.9210(17) . ?
Mo4 O12 1.9210(17) 2_656 ?
Mo4 O14 2.3524(16) . ?
Mo4 O14 2.3524(16) 2_656 ?
Mn1 O1 1.918(2) 5_557 ?
Mn1 O1 1.918(2) . ?
Mn1 O2 2.0095(17) 6 ?
Mn1 O2 2.0095(17) 2_557 ?
Mn1 O2 2.0095(17) 5_557 ?
Mn1 O2 2.0095(17) . ?
Mn2 O14 1.9687(16) 6 ?
Mn2 O14 1.9687(16) . ?
Mn2 O14 1.9687(16) 5_656 ?
Mn2 O14 1.9687(16) 2_656 ?
Mn2 O8 2.002(2) 5_656 ?
Mn2 O8 2.002(2) . ?
O1 C1 1.441(4) . ?
O1 Mo1 2.3629(16) 6 ?
O2 C2 1.440(3) . ?
O6 Mo1 1.9094(12) 6 ?
O8 C5 1.428(4) . ?
O8 Mo3 2.3543(16) 6 ?
O9 Mo3 1.9123(12) 6 ?
O14 C4 1.446(3) . ?
N1 C3 1.487(5) . ?
N2 C6 1.473(5) . ?
N3 C13 1.505(4) . ?
N3 C9 1.508(4) . ?
N3 C7 1.524(4) . ?
N3 C11 1.525(4) . ?
C1 C3 1.540(5) . ?
C2 C3 1.539(3) 5_557 ?
C3 C2 1.539(3) 5_557 ?
C3 C2 1.539(3) 2_557 ?
C4 C6 1.528(3) . ?
C5 C6 1.544(5) 5_656 ?
C6 C4 1.528(3) 6 ?
C6 C5 1.544(5) 5_656 ?
C7 C8 1.499(5) . ?
C9 C10 1.518(5) . ?
C11 C12 1.495(5) . ?
C13 C14 1.522(5) . ?
N4 C17' 1.40(3) 5_556 ?
N4 C17' 1.40(3) . ?
N4 C17 1.522(18) 5_556 ?
N4 C17 1.522(18) 6 ?
N4 C17 1.522(18) 2_556 ?
N4 C17 1.522(18) . ?
N4 C19 1.64(2) 6 ?
N4 C19 1.64(2) . ?
N4 C19 1.64(2) 5_556 ?
N4 C19 1.64(2) 2_556 ?
C15 C16 0.647(10) 6 ?
C15 C16 0.647(10) . ?
C15 C17 1.598(19) 6 ?
C15 C17 1.598(19) . ?
C15 C17' 1.60(3) . ?
C16 C16 1.286(19) 6 ?
C16 C17 1.42(2) . ?
C16 C17' 1.67(3) . ?
C16 C17 1.88(2) 6 ?
C17 C17 1.18(3) 6 ?
C17 C19 1.51(3) . ?
C17 C17' 1.57(3) . ?
C17 C18 1.76(3) . ?
C17 C16 1.88(2) 6 ?
C17 C19 2.00(3) 6 ?
C17' C19 1.50(3) 5_556 ?
C17' C19 1.50(3) 2_556 ?
C17' C17 1.57(3) 6 ?
C17' C16 1.67(3) 6 ?
C18 C19 1.37(3) . ?
C18 C18 1.44(5) 2_556 ?
C19 C19 1.45(4) 6 ?
C19 C17' 1.50(3) 5_556 ?
C19 C17 2.00(3) 6 ?
N5 C20 1.452(15) . ?
N5 C20 1.452(15) 2_655 ?
N5 C21 1.473(17) . ?
O15 C20 1.163(15) . ?
 
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
O7 Mo1 O5 105.20(12) . . ?
O7 Mo1 O6 98.60(11) . . ?
O5 Mo1 O6 101.98(12) . . ?
O7 Mo1 O4 103.06(11) . . ?
O5 Mo1 O4 97.89(11) . . ?
O6 Mo1 O4 145.49(10) . . ?
O7 Mo1 O2 93.88(9) . . ?
O5 Mo1 O2 160.09(9) . . ?
O6 Mo1 O2 80.31(9) . . ?
O4 Mo1 O2 71.77(7) . . ?
O7 Mo1 O1 162.57(10) . . ?
O5 Mo1 O1 90.97(10) . . ?
O6 Mo1 O1 71.14(8) . . ?
O4 Mo1 O1 80.65(7) . . ?
O2 Mo1 O1 70.88(7) . . ?
O3 Mo2 O3 105.77(17) . 2_557 ?
O3 Mo2 O4 101.57(12) . 2_557 ?
O3 Mo2 O4 99.49(12) 2_557 2_557 ?
O3 Mo2 O4 99.49(12) . . ?
O3 Mo2 O4 101.57(12) 2_557 . ?
O4 Mo2 O4 144.75(12) 2_557 . ?
O3 Mo2 O2 161.79(9) . . ?
O3 Mo2 O2 91.61(10) 2_557 . ?
O4 Mo2 O2 80.39(8) 2_557 . ?
O4 Mo2 O2 71.11(7) . . ?
O3 Mo2 O2 91.61(10) . 2_557 ?
O3 Mo2 O2 161.79(9) 2_557 2_557 ?
O4 Mo2 O2 71.11(7) 2_557 2_557 ?
O4 Mo2 O2 80.39(8) . 2_557 ?
O2 Mo2 O2 71.73(8) . 2_557 ?
O11 Mo3 O10 105.62(9) . . ?
O11 Mo3 O12 101.69(8) . . ?
O10 Mo3 O12 99.57(8) . . ?
O11 Mo3 O9 98.79(9) . . ?
O10 Mo3 O9 101.79(9) . . ?
O12 Mo3 O9 145.05(8) . . ?
O11 Mo3 O14 91.79(8) . . ?
O10 Mo3 O14 161.87(8) . . ?
O12 Mo3 O14 71.34(6) . . ?
O9 Mo3 O14 80.05(8) . . ?
O11 Mo3 O8 161.55(9) . . ?
O10 Mo3 O8 91.78(8) . . ?
O12 Mo3 O8 80.94(6) . . ?
O9 Mo3 O8 71.10(7) . . ?
O14 Mo3 O8 71.58(7) . . ?
O13 Mo4 O13 105.80(13) . 2_656 ?
O13 Mo4 O12 101.88(8) . . ?
O13 Mo4 O12 98.79(8) 2_656 . ?
O13 Mo4 O12 98.79(8) . 2_656 ?
O13 Mo4 O12 101.88(8) 2_656 2_656 ?
O12 Mo4 O12 145.41(10) . 2_656 ?
O13 Mo4 O14 92.33(7) . . ?
O13 Mo4 O14 160.94(7) 2_656 . ?
O12 Mo4 O14 71.16(6) . . ?
O12 Mo4 O14 80.62(6) 2_656 . ?
O13 Mo4 O14 160.94(8) . 2_656 ?
O13 Mo4 O14 92.33(7) 2_656 2_656 ?
O12 Mo4 O14 80.62(6) . 2_656 ?
O12 Mo4 O14 71.16(6) 2_656 2_656 ?
O14 Mo4 O14 70.39(8) . 2_656 ?
O1 Mn1 O1 180.0 5_557 . ?
O1 Mn1 O2 92.35(7) 5_557 6 ?
O1 Mn1 O2 87.65(7) . 6 ?
O1 Mn1 O2 87.65(7) 5_557 2_557 ?
O1 Mn1 O2 92.35(7) . 2_557 ?
O2 Mn1 O2 180.0 6 2_557 ?
O1 Mn1 O2 87.65(7) 5_557 5_557 ?
O1 Mn1 O2 92.35(7) . 5_557 ?
O2 Mn1 O2 87.17(10) 6 5_557 ?
O2 Mn1 O2 92.83(10) 2_557 5_557 ?
O1 Mn1 O2 92.35(7) 5_557 . ?
O1 Mn1 O2 87.65(7) . . ?
O2 Mn1 O2 92.83(10) 6 . ?
O2 Mn1 O2 87.17(10) 2_557 . ?
O2 Mn1 O2 180.0 5_557 . ?
O14 Mn2 O14 92.95(9) 6 . ?
O14 Mn2 O14 87.05(9) 6 5_656 ?
O14 Mn2 O14 180.00(9) . 5_656 ?
O14 Mn2 O14 180.00(6) 6 2_656 ?
O14 Mn2 O14 87.05(9) . 2_656 ?
O14 Mn2 O14 92.95(9) 5_656 2_656 ?
O14 Mn2 O8 92.27(6) 6 5_656 ?
O14 Mn2 O8 92.27(6) . 5_656 ?
O14 Mn2 O8 87.73(6) 5_656 5_656 ?
O14 Mn2 O8 87.73(7) 2_656 5_656 ?
O14 Mn2 O8 87.73(7) 6 . ?
O14 Mn2 O8 87.73(6) . . ?
O14 Mn2 O8 92.27(6) 5_656 . ?
O14 Mn2 O8 92.27(6) 2_656 . ?
O8 Mn2 O8 180.0 5_656 . ?
C1 O1 Mn1 117.78(19) . . ?
C1 O1 Mo1 120.58(11) . 6 ?
Mn1 O1 Mo1 101.53(7) . 6 ?
C1 O1 Mo1 120.58(11) . . ?
Mn1 O1 Mo1 101.53(7) . . ?
Mo1 O1 Mo1 89.68(8) 6 . ?
C2 O2 Mn1 115.98(15) . . ?
C2 O2 Mo1 121.30(15) . . ?
Mn1 O2 Mo1 99.94(7) . . ?
C2 O2 Mo2 122.89(15) . . ?
Mn1 O2 Mo2 100.55(7) . . ?
Mo1 O2 Mo2 91.01(6) . . ?
Mo2 O4 Mo1 121.03(10) . . ?
Mo1 O6 Mo1 121.52(13) . 6 ?
C5 O8 Mn2 116.24(19) . . ?
C5 O8 Mo3 122.54(11) . 6 ?
Mn2 O8 Mo3 99.79(8) . 6 ?
C5 O8 Mo3 122.54(11) . . ?
Mn2 O8 Mo3 99.79(8) . . ?
Mo3 O8 Mo3 90.45(8) 6 . ?
Mo3 O9 Mo3 121.83(13) . 6 ?
Mo3 O12 Mo4 121.49(9) . . ?
C4 O14 Mn2 116.09(14) . . ?
C4 O14 Mo3 121.73(14) . . ?
Mn2 O14 Mo3 100.90(7) . . ?
C4 O14 Mo4 121.34(14) . . ?
Mn2 O14 Mo4 101.28(7) . . ?
Mo3 O14 Mo4 90.61(6) . . ?
C13 N3 C9 108.6(2) . . ?
C13 N3 C7 112.3(2) . . ?
C9 N3 C7 106.0(2) . . ?
C13 N3 C11 108.7(2) . . ?
C9 N3 C11 111.2(2) . . ?
C7 N3 C11 110.0(2) . . ?
O1 C1 C3 113.0(3) . . ?
O2 C2 C3 113.1(2) . 5_557 ?
N1 C3 C2 107.07(19) . 5_557 ?
N1 C3 C2 107.07(19) . 2_557 ?
C2 C3 C2 113.0(3) 5_557 2_557 ?
N1 C3 C1 104.4(3) . . ?
C2 C3 C1 112.34(19) 5_557 . ?
C2 C3 C1 112.34(19) 2_557 . ?
O14 C4 C6 114.4(2) . . ?
O8 C5 C6 114.0(3) . 5_656 ?
N2 C6 C4 107.5(2) . 6 ?
N2 C6 C4 107.5(2) . . ?
C4 C6 C4 112.8(3) 6 . ?
N2 C6 C5 105.7(3) . 5_656 ?
C4 C6 C5 111.47(19) 6 5_656 ?
C4 C6 C5 111.5(2) . 5_656 ?
C8 C7 N3 115.2(3) . . ?
N3 C9 C10 114.3(3) . . ?
C12 C11 N3 115.3(3) . . ?
N3 C13 C14 115.0(3) . . ?
C17' N4 C17' 180.0 5_556 . ?
C17' N4 C17 65.1(12) 5_556 5_556 ?
C17' N4 C17 114.9(12) . 5_556 ?
C17' N4 C17 114.9(12) 5_556 6 ?
C17' N4 C17 65.1(12) . 6 ?
C17 N4 C17 134.3(13) 5_556 6 ?
C17' N4 C17 65.1(12) 5_556 2_556 ?
C17' N4 C17 114.9(12) . 2_556 ?
C17 N4 C17 45.7(13) 5_556 2_556 ?
C17 N4 C17 180.0(8) 6 2_556 ?
C17' N4 C17 114.9(12) 5_556 . ?
C17' N4 C17 65.1(12) . . ?
C17 N4 C17 180.000(3) 5_556 . ?
C17 N4 C17 45.7(13) 6 . ?
C17 N4 C17 134.3(13) 2_556 . ?
C17' N4 C19 58.4(11) 5_556 6 ?
C17' N4 C19 121.6(11) . 6 ?
C17 N4 C19 101.8(10) 5_556 6 ?
C17 N4 C19 56.8(10) 6 6 ?
C17 N4 C19 123.2(10) 2_556 6 ?
C17 N4 C19 78.2(10) . 6 ?
C17' N4 C19 58.4(11) 5_556 . ?
C17' N4 C19 121.6(11) . . ?
C17 N4 C19 123.2(10) 5_556 . ?
C17 N4 C19 78.2(10) 6 . ?
C17 N4 C19 101.8(10) 2_556 . ?
C17 N4 C19 56.8(10) . . ?
C19 N4 C19 52.4(14) 6 . ?
C17' N4 C19 121.6(11) 5_556 5_556 ?
C17' N4 C19 58.4(11) . 5_556 ?
C17 N4 C19 56.8(10) 5_556 5_556 ?
C17 N4 C19 101.8(10) 6 5_556 ?
C17 N4 C19 78.2(10) 2_556 5_556 ?
C17 N4 C19 123.2(10) . 5_556 ?
C19 N4 C19 127.6(14) 6 5_556 ?
C19 N4 C19 180.0(10) . 5_556 ?
C17' N4 C19 121.6(11) 5_556 2_556 ?
C17' N4 C19 58.4(11) . 2_556 ?
C17 N4 C19 78.2(10) 5_556 2_556 ?
C17 N4 C19 123.2(10) 6 2_556 ?
C17 N4 C19 56.8(10) 2_556 2_556 ?
C17 N4 C19 101.8(10) . 2_556 ?
C19 N4 C19 180.000(3) 6 2_556 ?
C19 N4 C19 127.6(14) . 2_556 ?
C19 N4 C19 52.4(14) 5_556 2_556 ?
C16 C15 C16 167(2) 6 . ?
C16 C15 C17 62.3(13) 6 6 ?
C16 C15 C17 105.6(14) . 6 ?
C16 C15 C17 105.6(14) 6 . ?
C16 C15 C17 62.3(13) . . ?
C17 C15 C17 43.4(13) 6 . ?
C16 C15 C17' 85.0(12) 6 . ?
C16 C15 C17' 85.0(12) . . ?
C17 C15 C17' 59.0(11) 6 . ?
C17 C15 C17' 59.0(11) . . ?
C15 C16 C16 6.4(12) . 6 ?
C15 C16 C17 93.9(14) . . ?
C16 C16 C17 87.9(8) 6 . ?
C15 C16 C17' 72.4(12) . . ?
C16 C16 C17' 67.4(5) 6 . ?
C17 C16 C17' 60.6(12) . . ?
C15 C16 C17 55.0(12) . 6 ?
C16 C16 C17 49.0(6) 6 6 ?
C17 C16 C17 38.9(12) . 6 ?
C17' C16 C17 52.2(10) . 6 ?
C17 C17 C16 92.1(8) 6 . ?
C17 C17 C19 95.1(10) 6 . ?
C16 C17 C19 171.6(16) . . ?
C17 C17 N4 67.2(7) 6 . ?
C16 C17 N4 121.5(13) . . ?
C19 C17 N4 65.6(11) . . ?
C17 C17 C17' 68.0(7) 6 . ?
C16 C17 C17' 67.7(13) . . ?
C19 C17 C17' 119.1(17) . . ?
N4 C17 C17' 53.8(11) . . ?
C17 C17 C15 68.3(6) 6 . ?
C16 C17 C15 23.8(5) . . ?
C19 C17 C15 162.6(15) . . ?
N4 C17 C15 109.9(11) . . ?
C17' C17 C15 60.6(12) . . ?
C17 C17 C18 136.3(10) 6 . ?
C16 C17 C18 126.5(15) . . ?
C19 C17 C18 48.7(12) . . ?
N4 C17 C18 74.6(11) . . ?
C17' C17 C18 105.3(15) . . ?
C15 C17 C18 148.2(14) . . ?
C17 C17 C16 49.0(6) 6 6 ?
C16 C17 C16 43.1(8) . 6 ?
C19 C17 C16 143.8(14) . 6 ?
N4 C17 C16 97.4(10) . 6 ?
C17' C17 C16 57.1(10) . 6 ?
C15 C17 C16 19.4(4) . 6 ?
C18 C17 C16 160.8(14) . 6 ?
C17 C17 C19 48.8(8) 6 6 ?
C16 C17 C19 140.7(13) . 6 ?
C19 C17 C19 46.3(13) . 6 ?
N4 C17 C19 53.6(8) . 6 ?
C17' C17 C19 95.4(12) . 6 ?
C15 C17 C19 116.9(11) . 6 ?
C18 C17 C19 91.5(13) . 6 ?
C16 C17 C19 97.7(10) 6 6 ?
N4 C17' C19 68.8(14) . 5_556 ?
N4 C17' C19 68.8(14) . 2_556 ?
C19 C17' C19 57.8(18) 5_556 2_556 ?
N4 C17' C17 61.2(12) . 6 ?
C19 C17' C17 106.1(15) 5_556 6 ?
C19 C17' C17 130(2) 2_556 6 ?
N4 C17' C17 61.2(12) . . ?
C19 C17' C17 130(2) 5_556 . ?
C19 C17' C17 106.1(15) 2_556 . ?
C17 C17' C17 44.0(15) 6 . ?
N4 C17' C15 116.5(18) . . ?
C19 C17' C15 151.0(9) 5_556 . ?
C19 C17' C15 151.0(9) 2_556 . ?
C17 C17' C15 60.4(12) 6 . ?
C17 C17' C15 60.4(12) . . ?
N4 C17' C16 112.9(16) . . ?
C19 C17' C16 173.7(12) 5_556 . ?
C19 C17' C16 128.5(8) 2_556 . ?
C17 C17' C16 70.6(13) 6 . ?
C17 C17' C16 51.7(10) . . ?
C15 C17' C16 22.6(5) . . ?
N4 C17' C16 112.9(16) . 6 ?
C19 C17' C16 128.5(8) 5_556 6 ?
C19 C17' C16 173.7(12) 2_556 6 ?
C17 C17' C16 51.7(10) 6 6 ?
C17 C17' C16 70.6(13) . 6 ?
C15 C17' C16 22.6(5) . 6 ?
C16 C17' C16 45.2(10) . 6 ?
C19 C18 C18 123.4(14) . 2_556 ?
C19 C18 C17 56.1(13) . . ?
C18 C18 C17 89.5(17) 2_556 . ?
C18 C19 C19 146.4(13) . 6 ?
C18 C19 C17' 100.5(18) . 5_556 ?
C19 C19 C17' 61.1(9) 6 5_556 ?
C18 C19 C17 75.2(16) . . ?
C19 C19 C17 84.9(10) 6 . ?
C17' C19 C17 110.1(17) 5_556 . ?
C18 C19 N4 82.6(15) . . ?
C19 C19 N4 63.8(7) 6 . ?
C17' C19 N4 52.8(12) 5_556 . ?
C17 C19 N4 57.6(10) . . ?
C18 C19 C17 107.5(17) . 6 ?
C19 C19 C17 48.8(8) 6 6 ?
C17' C19 C17 88.5(13) 5_556 6 ?
C17 C19 C17 36.1(12) . 6 ?
N4 C19 C17 48.3(7) . 6 ?
C20 N5 C20 123.4(14) . 2_655 ?
C20 N5 C21 118.3(7) . . ?
C20 N5 C21 118.3(7) 2_655 . ?
O15 C20 N5 137.4(12) . . ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              26.00
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    1.41 
_refine_diff_density_min   -1.29 
_refine_diff_density_rms    0.14 
