# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_contact_author_name 'Dr Theocharis Stamatatos'
_publ_contact_author_email thstama@chemistry.upatras.gr
loop_
_publ_author_name
'Dimitris Alexandropoulos'
'Constantina Papatriantafyllopoulou'
'Shreya Mukherjee'
'Emmanouil Manos'
'Anastasios Tasiopoulos'
'Spyros Perlepes'
'George Christou'
'Theocharis Stamatatos'
data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 860119'
#TrackingRef '- Re-Revised Compound 2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C96 H72 Mn4 N16 Ni4 O20, 4(Cl O4), 4(C H2 Cl2), 21.5(H2 O)'
_chemical_formula_sum 'C100 H123 Cl8 Mn4 N16 Ni4 O57.50'
_chemical_formula_weight 3207.34
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Tetragonal
_symmetry_space_group_name_H-M 'I -4 2 m '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
_cell_length_a 16.7927(8)
_cell_length_b 16.7927(8)
_cell_length_c 25.9583(10)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 7320.1(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 2600
_cell_measurement_theta_min 2.8836
_cell_measurement_theta_max 24.9940
_exptl_crystal_description polyhedral
_exptl_crystal_colour red
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.04
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.455
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3286
_exptl_absorpt_coefficient_mu 1.071
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.36199
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator mirror
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9559
_diffrn_reflns_av_R_equivalents 0.0742
_diffrn_reflns_av_sigmaI/netI 0.0828
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 2.89
_diffrn_reflns_theta_max 25.00
_reflns_number_total 3380
_reflns_number_gt 2391
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis CCD'
_computing_cell_refinement 'CrysAlis RED'
_computing_data_reduction 'CrysAlis RED'
_computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
MERCURY (Bruno et al. 2002)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435--436.
Farrugia, L. J. (1997). ORTEP-3 for Windows. J.Appl. Cryst.
30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_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.
We have put restraints to limit the disorder of the oxygen atoms of ClO4 anions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.21(4)
_refine_ls_number_reflns 3380
_refine_ls_number_parameters 189
_refine_ls_number_restraints 18
_refine_ls_R_factor_all 0.0946
_refine_ls_R_factor_gt 0.0751
_refine_ls_wR_factor_ref 0.2120
_refine_ls_wR_factor_gt 0.1964
_refine_ls_goodness_of_fit_ref 1.002
_refine_ls_restrained_S_all 1.020
_refine_ls_shift/su_max 0.000
_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
Ni1 Ni 0.27665(9) 0.0000 0.0000 0.0498(4) Uani 1 2 d S . .
Mn1 Mn 0.15474(8) -0.15474(8) 0.02406(5) 0.0523(5) Uani 1 2 d S . .
Cl1 Cl 0.1786(2) 0.8214(2) 0.85568(10) 0.0894(13) Uani 1 2 d S . .
O1 O 0.1875(4) -0.0760(3) -0.02285(18) 0.0620(15) Uani 1 1 d . . .
O2 O 0.2271(4) -0.1216(4) 0.07832(18) 0.0660(17) Uani 1 1 d . . .
O3 O 0.2414(4) -0.2414(4) -0.0086(3) 0.072(2) Uani 1 2 d S . .
O4 O 0.1195(13) 0.8805(13) 0.8660(11) 0.248(7) Uani 1 2 d SU . .
O5 O 0.1810(4) 0.8190(4) 0.8017(3) 0.077(2) Uani 1 2 d SU . .
O6 O 0.2306(6) 0.8691(6) 0.8729(3) 0.119(3) Uani 1 1 d U . .
N1 N 0.2750(4) -0.0608(4) 0.0670(2) 0.0530(16) Uani 1 1 d . . .
N2 N 0.3617(4) 0.0638(4) 0.0427(2) 0.0489(16) Uani 1 1 d . . .
C1 C 0.3236(6) -0.0344(4) 0.1051(3) 0.055(2) Uani 1 1 d . . .
C2 C 0.3202(4) -0.0677(4) 0.1575(2) 0.0368(15) Uani 1 1 d . . .
C3 C 0.3334(5) -0.1500(5) 0.1654(3) 0.055(2) Uani 1 1 d . . .
H3 H 0.3434 -0.1838 0.1378 0.066 Uiso 1 1 calc R . .
C4 C 0.3310(5) -0.1783(5) 0.2140(2) 0.057(2) Uani 1 1 d . . .
H4 H 0.3401 -0.2323 0.2193 0.068 Uiso 1 1 calc R . .
C5 C 0.3153(6) -0.1296(6) 0.2568(3) 0.067(3) Uani 1 1 d . . .
H5 H 0.3105 -0.1515 0.2895 0.080 Uiso 1 1 calc R . .
C6 C 0.3070(6) -0.0486(6) 0.2493(3) 0.068(3) Uani 1 1 d . . .
H6 H 0.3039 -0.0142 0.2773 0.082 Uiso 1 1 calc R . .
C7 C 0.3032(6) -0.0190(6) 0.1990(3) 0.072(3) Uani 1 1 d . . .
H7 H 0.2892 0.0339 0.1934 0.086 Uiso 1 1 calc R . .
C8 C 0.3692(5) 0.0344(5) 0.0890(3) 0.055(2) Uani 1 1 d . . .
C9 C 0.3980(5) 0.1265(5) 0.0286(3) 0.053(2) Uani 1 1 d . . .
H9 H 0.3862 0.1468 -0.0038 0.063 Uiso 1 1 calc R . .
C10 C 0.4552(6) 0.1682(6) 0.0586(3) 0.064(2) Uani 1 1 d . . .
H10 H 0.4831 0.2120 0.0461 0.077 Uiso 1 1 calc R . .
C11 C 0.4664(5) 0.1378(5) 0.1087(3) 0.059(2) Uani 1 1 d . . .
H11 H 0.5018 0.1624 0.1312 0.071 Uiso 1 1 calc R . .
C12 C 0.4243(6) 0.0708(6) 0.1242(3) 0.067(3) Uani 1 1 d . . .
H12 H 0.4316 0.0498 0.1570 0.081 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
Ni1 0.0867(10) 0.0471(7) 0.0156(5) -0.0001(6) 0.000 0.000
Mn1 0.0693(7) 0.0693(7) 0.0184(6) 0.0045(5) -0.0045(5) -0.0019(9)
Cl1 0.115(2) 0.115(2) 0.0380(14) -0.0284(14) 0.0284(14) -0.056(3)
O1 0.099(4) 0.060(3) 0.027(2) 0.002(2) -0.022(3) -0.005(3)
O2 0.104(5) 0.067(4) 0.027(2) 0.004(2) -0.022(3) -0.026(3)
O3 0.079(3) 0.079(3) 0.058(5) -0.006(3) 0.006(3) 0.009(4)
O4 0.251(7) 0.251(7) 0.244(9) -0.002(4) 0.002(4) 0.008(5)
O5 0.089(3) 0.089(3) 0.054(3) -0.009(3) 0.009(3) -0.012(4)
O6 0.130(5) 0.133(5) 0.094(4) -0.006(4) -0.003(4) -0.036(4)
N1 0.075(5) 0.060(4) 0.024(3) -0.010(3) -0.008(3) -0.009(4)
N2 0.075(4) 0.054(4) 0.017(2) -0.003(3) 0.005(3) -0.013(3)
C1 0.087(6) 0.041(4) 0.036(4) -0.003(3) -0.024(4) 0.011(4)
C2 0.049(4) 0.038(4) 0.023(3) 0.001(3) -0.003(3) 0.000(3)
C3 0.080(6) 0.052(5) 0.034(3) -0.004(3) -0.010(4) -0.019(4)
C4 0.084(6) 0.052(5) 0.035(3) 0.014(3) -0.021(4) -0.010(4)
C5 0.080(6) 0.085(7) 0.034(4) 0.006(4) -0.025(4) -0.010(5)
C6 0.101(7) 0.072(6) 0.032(4) -0.006(4) 0.001(4) -0.016(5)
C7 0.112(7) 0.087(7) 0.018(3) 0.008(4) -0.017(4) -0.002(6)
C8 0.067(6) 0.063(5) 0.036(4) 0.001(4) -0.008(4) -0.010(4)
C9 0.078(6) 0.053(5) 0.027(4) -0.009(4) -0.002(4) 0.000(4)
C10 0.088(6) 0.077(6) 0.028(3) -0.007(4) 0.028(4) -0.010(5)
C11 0.064(5) 0.065(6) 0.050(4) -0.016(4) -0.004(4) -0.010(4)
C12 0.101(8) 0.078(6) 0.022(3) -0.006(4) 0.004(4) -0.010(5)
_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
Ni1 N1 2.017(6) . ?
Ni1 N1 2.017(6) 3 ?
Ni1 O1 2.055(6) . ?
Ni1 O1 2.055(6) 3 ?
Ni1 N2 2.101(6) 3 ?
Ni1 N2 2.101(6) . ?
Mn1 O1 1.879(5) . ?
Mn1 O1 1.879(5) 6 ?
Mn1 O2 1.942(5) . ?
Mn1 O2 1.942(5) 6 ?
Mn1 O3 2.225(9) . ?
Cl1 O6 1.266(9) 6_665 ?
Cl1 O6 1.267(9) . ?
Cl1 O5 1.403(8) . ?
Cl1 O4 1.43(3) . ?
O2 N1 1.333(9) . ?
N1 C1 1.355(9) . ?
N2 C9 1.270(10) . ?
N2 C8 1.306(9) . ?
C1 C8 1.448(12) . ?
C1 C2 1.473(10) . ?
C2 C7 1.383(11) . ?
C2 C3 1.414(10) . ?
C3 C4 1.347(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.398(11) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C12 1.437(11) . ?
C9 C10 1.420(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.410(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(12) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
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
N1 Ni1 N1 178.4(4) . 3 ?
N1 Ni1 O1 85.7(2) . . ?
N1 Ni1 O1 93.2(2) 3 . ?
N1 Ni1 O1 93.2(2) . 3 ?
N1 Ni1 O1 85.7(2) 3 3 ?
O1 Ni1 O1 86.5(3) . 3 ?
N1 Ni1 N2 101.9(3) . 3 ?
N1 Ni1 N2 79.2(2) 3 3 ?
O1 Ni1 N2 91.5(2) . 3 ?
O1 Ni1 N2 164.6(2) 3 3 ?
N1 Ni1 N2 79.2(2) . . ?
N1 Ni1 N2 101.9(3) 3 . ?
O1 Ni1 N2 164.6(2) . . ?
O1 Ni1 N2 91.5(2) 3 . ?
N2 Ni1 N2 94.3(3) 3 . ?
O1 Mn1 O1 89.6(3) . 6 ?
O1 Mn1 O2 94.9(2) . . ?
O1 Mn1 O2 173.7(2) 6 . ?
O1 Mn1 O2 173.7(2) . 6 ?
O1 Mn1 O2 94.9(2) 6 6 ?
O2 Mn1 O2 80.3(3) . 6 ?
O1 Mn1 O3 91.2(2) . . ?
O1 Mn1 O3 91.2(2) 6 . ?
O2 Mn1 O3 93.1(3) . . ?
O2 Mn1 O3 93.1(3) 6 . ?
O6 Cl1 O6 138.5(8) 6_665 . ?
O6 Cl1 O5 110.5(4) 6_665 . ?
O6 Cl1 O5 110.5(4) . . ?
O6 Cl1 O4 88.5(6) 6_665 . ?
O6 Cl1 O4 88.5(6) . . ?
O5 Cl1 O4 103.2(13) . . ?
Mn1 O1 Ni1 117.6(2) . . ?
N1 O2 Mn1 115.9(4) . . ?
O2 N1 C1 116.9(6) . . ?
O2 N1 Ni1 125.9(4) . . ?
C1 N1 Ni1 117.1(5) . . ?
C9 N2 C8 122.1(7) . . ?
C9 N2 Ni1 126.7(5) . . ?
C8 N2 Ni1 110.9(6) . . ?
N1 C1 C8 111.7(7) . . ?
N1 C1 C2 121.8(7) . . ?
C8 C1 C2 126.1(7) . . ?
C7 C2 C3 119.8(6) . . ?
C7 C2 C1 120.2(6) . . ?
C3 C2 C1 120.0(6) . . ?
C4 C3 C2 118.4(7) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 122.7(8) . . ?
C3 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C6 C5 C4 118.7(7) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 119.1(8) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C2 C7 C6 120.5(9) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N2 C8 C12 119.1(8) . . ?
N2 C8 C1 121.1(7) . . ?
C12 C8 C1 119.8(7) . . ?
N2 C9 C10 125.2(7) . . ?
N2 C9 H9 117.4 . . ?
C10 C9 H9 117.4 . . ?
C11 C10 C9 114.7(8) . . ?
C11 C10 H10 122.7 . . ?
C9 C10 H10 122.7 . . ?
C12 C11 C10 119.5(8) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C8 119.3(7) . . ?
C11 C12 H12 120.4 . . ?
C8 C12 H12 120.4 . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.746
_refine_diff_density_min -0.529
_refine_diff_density_rms 0.104
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.004 1260 383 ' '
2 0.000 0.500 0.250 25 2 ' '
3 0.000 0.500 0.750 25 2 ' '
4 0.500 0.500 0.025 1260 383 ' '
5 0.500 0.000 0.250 25 2 ' '
6 0.500 1.000 0.750 25 2 ' '
# start Validation Reply Form
_vrf_CHEMW03_shelxl
;
RESPONSE: The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents (4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT051_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents (4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT043_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents (4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT041_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents(4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT042_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents(4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT068_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents(4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_FORMU01_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
_vrf_CELLZ01_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density, Mu etc include
the contribution of disordered solvents(4 CH2Cl2, 21.5 H2O),
which were removed by SQUEEZE.
;
# end Validation Reply Form
# Attachment '- Re-revised Compound 1.cif'
data_shelxl2
_database_code_depnum_ccdc_archive 'CCDC 860120'
#TrackingRef '- Re-revised Compound 1.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C144 H108 Mn12 N24 O24, 3(Cl O4), 6(C2 H3 N), H O, 6(H2 O)'
_chemical_formula_sum 'C156 H121 Cl3 Mn12 N30 O34'
_chemical_formula_weight 3725.46
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
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 17.9483(3)
_cell_length_b 21.9148(3)
_cell_length_c 21.9379(4)
_cell_angle_alpha 90.00
_cell_angle_beta 98.882(2)
_cell_angle_gamma 90.00
_cell_volume 8525.4(2)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 25433
_cell_measurement_theta_min 2.7288
_cell_measurement_theta_max 29.2133
_exptl_crystal_description rod
_exptl_crystal_colour 'dark red'
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.451
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3780
_exptl_absorpt_coefficient_mu 0.981
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.51132
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator mirror
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 74336
_diffrn_reflns_av_R_equivalents 0.0575
_diffrn_reflns_av_sigmaI/netI 0.0601
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.73
_diffrn_reflns_theta_max 25.00
_reflns_number_total 14989
_reflns_number_gt 10832
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis CCD'
_computing_cell_refinement 'CrysAlis RED'
_computing_data_reduction 'CrysAlis RED'
_computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
MERCURY (Bruno et al. 2002)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435--436.
Farrugia, L. J. (1997). ORTEP-3 for Windows. J.Appl. Cryst.
30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_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.
We have put restraints to limit the disorder of the oxygen atoms of ClO4
and fix the position of H74.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 14989
_refine_ls_number_parameters 1083
_refine_ls_number_restraints 64
_refine_ls_R_factor_all 0.0592
_refine_ls_R_factor_gt 0.0428
_refine_ls_wR_factor_ref 0.1236
_refine_ls_wR_factor_gt 0.1187
_refine_ls_goodness_of_fit_ref 0.961
_refine_ls_restrained_S_all 0.974
_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
Mn1 Mn 0.17011(3) 0.43092(2) 0.89875(2) 0.01440(13) Uani 1 1 d . . .
Mn2 Mn 0.27287(3) 0.51624(2) 1.01956(2) 0.01227(13) Uani 1 1 d . . .
Mn3 Mn 0.13773(3) 0.42731(2) 1.06049(2) 0.01543(13) Uani 1 1 d . . .
Mn4 Mn 0.06032(3) 0.53822(2) 0.97104(2) 0.01088(12) Uani 1 1 d . . .
Mn5 Mn 0.14715(3) 0.62946(2) 1.02948(2) 0.01207(13) Uani 1 1 d . . .
Mn6 Mn -0.02189(3) 0.44792(2) 0.89760(2) 0.01234(13) Uani 1 1 d . . .
Cl1 Cl 0.33965(9) 0.29912(6) 1.07113(6) 0.0620(4) Uani 1 1 d . . .
Cl2 Cl 0.0371(2) 0.51996(17) 0.50397(16) 0.0825(10) Uani 0.50 1 d P . .
N1 N 0.15593(17) 0.46393(14) 0.79553(14) 0.0213(7) Uani 1 1 d . . .
N2 N 0.24334(16) 0.51066(12) 0.89082(13) 0.0159(6) Uani 1 1 d . . .
N3 N 0.22738(17) 0.34216(13) 0.88378(14) 0.0208(7) Uani 1 1 d . . .
N4 N 0.08164(16) 0.36195(13) 0.86603(13) 0.0183(7) Uani 1 1 d . . .
N5 N 0.40023(16) 0.51636(12) 1.04525(13) 0.0165(6) Uani 1 1 d . . .
N6 N 0.30407(15) 0.60819(12) 1.03954(13) 0.0143(6) Uani 1 1 d . . .
N7 N 0.14177(16) 0.37934(13) 1.15241(14) 0.0189(7) Uani 1 1 d . . .
N8 N 0.23694(16) 0.45888(12) 1.12387(13) 0.0146(6) Uani 1 1 d . . .
N9 N 0.13933(16) 0.72300(12) 1.03512(13) 0.0156(6) Uani 1 1 d . . .
N10 N 0.11530(15) 0.65383(12) 0.94109(13) 0.0139(6) Uani 1 1 d . . .
N11 N -0.04645(16) 0.49626(12) 0.80635(13) 0.0163(6) Uani 1 1 d . . .
N12 N -0.12981(16) 0.41914(12) 0.85581(13) 0.0143(6) Uani 1 1 d . . .
N13 N 0.1659(3) 0.9253(2) 0.7347(3) 0.0732(15) Uani 1 1 d . . .
O1 O 0.29404(13) 0.53015(10) 0.93935(11) 0.0181(5) Uani 1 1 d . . .
O2 O 0.00727(13) 0.37525(10) 0.85753(11) 0.0165(5) Uani 1 1 d . . .
O3 O 0.25210(13) 0.65323(10) 1.02776(11) 0.0161(5) Uani 1 1 d . . .
O4 O 0.28012(13) 0.50439(9) 1.10615(10) 0.0154(5) Uani 1 1 d . . .
O5 O 0.08641(13) 0.61123(10) 0.90261(10) 0.0164(5) Uani 1 1 d . . .
O6 O -0.16990(13) 0.37761(10) 0.88361(10) 0.0152(5) Uani 1 1 d . . .
O7 O 0.22538(13) 0.43583(9) 0.99788(11) 0.0149(5) Uani 1 1 d . . .
O8 O 0.07684(13) 0.47017(10) 0.92497(11) 0.0152(5) Uani 1 1 d . . .
O9 O 0.16417(12) 0.55185(9) 1.00698(11) 0.0132(5) Uani 1 1 d . . .
O10 O 0.04835(12) 0.60578(9) 1.02593(10) 0.0133(5) Uani 1 1 d . . .
O11 O 0.04486(12) 0.48158(9) 1.05614(10) 0.0120(5) Uani 1 1 d . . .
O12 O 0.08688(15) 0.34986(11) 1.01468(12) 0.0268(6) Uani 1 1 d . . .
O13A O 0.3106(5) 0.2434(2) 1.0375(4) 0.058(3) Uani 0.599(13) 1 d PU . .
O13B O 0.3556(8) 0.2462(5) 1.0786(7) 0.084(5) Uani 0.401(13) 1 d PU . .
O14A O 0.2560(9) 0.3132(6) 1.0723(8) 0.082(6) Uani 0.292(11) 1 d PU . .
O14B O 0.3075(5) 0.3110(3) 1.1216(3) 0.045(3) Uani 0.465(12) 1 d PU . .
O14C O 0.3622(8) 0.3431(6) 1.1294(5) 0.037(5) Uani 0.244(10) 1 d PU . .
O15 O 0.3398(2) 0.34583(15) 1.02749(17) 0.0594(10) Uani 1 1 d . . .
O16A O 0.4221(4) 0.2823(3) 1.0935(4) 0.103(3) Uani 0.703(11) 1 d PU . .
O16B O 0.4065(9) 0.3184(7) 1.0392(8) 0.084(7) Uani 0.296(11) 1 d PU . .
O17 O -0.0076(3) 0.5232(2) 0.5476(2) 0.0985(15) Uani 1 1 d U . .
O18 O 0.1134(6) 0.4968(5) 0.5261(5) 0.115(3) Uani 0.50 1 d PU . .
O19 O 0.0318(8) 0.5759(6) 0.4705(6) 0.141(4) Uani 0.50 1 d PU . .
O20 O 0.1518(3) 0.2436(2) 1.0033(3) 0.0422(16) Uani 0.50 1 d PD . .
C1 C 0.1096(2) 0.44012(19) 0.74760(18) 0.0295(10) Uani 1 1 d . . .
H1 H 0.0830 0.4049 0.7541 0.035 Uiso 1 1 calc R . .
C2 C 0.0990(3) 0.4652(2) 0.6889(2) 0.0390(11) Uani 1 1 d . . .
H2 H 0.0677 0.4464 0.6567 0.047 Uiso 1 1 calc R . .
C3 C 0.1358(3) 0.5182(2) 0.6796(2) 0.0425(12) Uani 1 1 d . . .
H3 H 0.1289 0.5365 0.6409 0.051 Uiso 1 1 calc R . .
C4 C 0.1836(2) 0.5447(2) 0.72882(19) 0.0330(10) Uani 1 1 d . . .
H4 H 0.2084 0.5811 0.7234 0.040 Uiso 1 1 calc R . .
C5 C 0.1936(2) 0.51589(17) 0.78595(17) 0.0212(8) Uani 1 1 d . . .
C6 C 0.2453(2) 0.53941(16) 0.83924(16) 0.0188(8) Uani 1 1 d . . .
C7 C 0.2956(2) 0.59249(17) 0.83437(17) 0.0229(9) Uani 1 1 d . . .
C8 C 0.3465(2) 0.59195(19) 0.79216(19) 0.0304(10) Uani 1 1 d . . .
H8 H 0.3484 0.5588 0.7660 0.037 Uiso 1 1 calc R . .
C9 C 0.3945(2) 0.6418(2) 0.7896(2) 0.0423(12) Uani 1 1 d . . .
H9 H 0.4280 0.6417 0.7613 0.051 Uiso 1 1 calc R . .
C10 C 0.3929(3) 0.6907(2) 0.8281(2) 0.0455(12) Uani 1 1 d . . .
H10 H 0.4256 0.7233 0.8261 0.055 Uiso 1 1 calc R . .
C11 C 0.3424(3) 0.69144(19) 0.8699(2) 0.0411(11) Uani 1 1 d . . .
H11 H 0.3409 0.7247 0.8960 0.049 Uiso 1 1 calc R . .
C12 C 0.2941(2) 0.64242(17) 0.87288(19) 0.0283(9) Uani 1 1 d . . .
H12 H 0.2604 0.6431 0.9011 0.034 Uiso 1 1 calc R . .
C13 C 0.3013(2) 0.33240(17) 0.89412(18) 0.0267(9) Uani 1 1 d . . .
H13 H 0.3325 0.3651 0.9077 0.032 Uiso 1 1 calc R . .
C14 C 0.3345(2) 0.27693(18) 0.8860(2) 0.0360(11) Uani 1 1 d . . .
H14 H 0.3866 0.2723 0.8944 0.043 Uiso 1 1 calc R . .
C15 C 0.2886(2) 0.22865(19) 0.8652(2) 0.0387(11) Uani 1 1 d . . .
H15 H 0.3092 0.1905 0.8597 0.046 Uiso 1 1 calc R . .
C16 C 0.2111(2) 0.23733(17) 0.8525(2) 0.0309(10) Uani 1 1 d . . .
H16 H 0.1793 0.2056 0.8370 0.037 Uiso 1 1 calc R . .
C17 C 0.1818(2) 0.29433(16) 0.86329(17) 0.0224(9) Uani 1 1 d . . .
C18 C 0.0994(2) 0.30705(16) 0.85374(17) 0.0200(8) Uani 1 1 d . . .
C19 C 0.0430(2) 0.25867(16) 0.83129(19) 0.0237(9) Uani 1 1 d . . .
C20 C 0.0398(2) 0.20529(17) 0.8648(2) 0.0358(11) Uani 1 1 d . . .
H20 H 0.0731 0.1995 0.9012 0.043 Uiso 1 1 calc R . .
C21 C -0.0124(3) 0.1609(2) 0.8445(3) 0.0473(13) Uani 1 1 d . . .
H21 H -0.0146 0.1253 0.8673 0.057 Uiso 1 1 calc R . .
C22 C -0.0604(3) 0.1692(2) 0.7915(3) 0.0538(16) Uani 1 1 d . . .
H22 H -0.0947 0.1385 0.7776 0.065 Uiso 1 1 calc R . .
C23 C -0.0597(3) 0.2217(2) 0.7577(3) 0.0518(15) Uani 1 1 d . . .
H23 H -0.0936 0.2269 0.7215 0.062 Uiso 1 1 calc R . .
C24 C -0.0070(2) 0.26762(19) 0.7783(2) 0.0370(11) Uani 1 1 d . . .
H24 H -0.0063 0.3038 0.7562 0.044 Uiso 1 1 calc R . .
C25 C 0.4457(2) 0.46788(16) 1.05388(17) 0.0203(8) Uani 1 1 d . . .
H25 H 0.4265 0.4301 1.0400 0.024 Uiso 1 1 calc R . .
C26 C 0.5192(2) 0.47105(16) 1.08217(18) 0.0220(8) Uani 1 1 d . . .
H26 H 0.5492 0.4363 1.0869 0.026 Uiso 1 1 calc R . .
C27 C 0.5477(2) 0.52701(17) 1.10354(18) 0.0246(9) Uani 1 1 d . . .
H27 H 0.5970 0.5305 1.1238 0.030 Uiso 1 1 calc R . .
C28 C 0.5017(2) 0.57760(16) 1.09419(17) 0.0193(8) Uani 1 1 d . . .
H28 H 0.5198 0.6157 1.1080 0.023 Uiso 1 1 calc R . .
C29 C 0.42808(19) 0.57148(15) 1.06404(16) 0.0174(8) Uani 1 1 d . . .
C30 C 0.37465(19) 0.62351(15) 1.05325(16) 0.0167(8) Uani 1 1 d . . .
C31 C 0.4018(2) 0.68767(15) 1.05839(17) 0.0196(8) Uani 1 1 d . . .
C32 C 0.3730(2) 0.72928(17) 1.0962(2) 0.0317(10) Uani 1 1 d . . .
H32 H 0.3356 0.7172 1.1187 0.038 Uiso 1 1 calc R . .
C33 C 0.3996(3) 0.78895(19) 1.1008(2) 0.0448(12) Uani 1 1 d . . .
H33 H 0.3804 0.8165 1.1266 0.054 Uiso 1 1 calc R . .
C34 C 0.4543(3) 0.80750(19) 1.0671(2) 0.0428(12) Uani 1 1 d . . .
H34 H 0.4720 0.8475 1.0702 0.051 Uiso 1 1 calc R . .
C35 C 0.4826(2) 0.76676(18) 1.0290(2) 0.0352(11) Uani 1 1 d . . .
H35 H 0.5191 0.7793 1.0059 0.042 Uiso 1 1 calc R . .
C36 C 0.4569(2) 0.70664(17) 1.02477(18) 0.0257(9) Uani 1 1 d . . .
H36 H 0.4769 0.6792 0.9993 0.031 Uiso 1 1 calc R . .
C37 C 0.0929(2) 0.33608(16) 1.16347(18) 0.0229(9) Uani 1 1 d . . .
H37 H 0.0481 0.3319 1.1362 0.027 Uiso 1 1 calc R . .
C38 C 0.1062(2) 0.29735(17) 1.21358(19) 0.0296(10) Uani 1 1 d . . .
H38 H 0.0706 0.2685 1.2207 0.036 Uiso 1 1 calc R . .
C39 C 0.1738(2) 0.30257(17) 1.25294(19) 0.0314(10) Uani 1 1 d . . .
H39 H 0.1854 0.2758 1.2860 0.038 Uiso 1 1 calc R . .
C40 C 0.2241(2) 0.34781(16) 1.24294(18) 0.0250(9) Uani 1 1 d . . .
H40 H 0.2698 0.3520 1.2691 0.030 Uiso 1 1 calc R . .
C41 C 0.2054(2) 0.38698(15) 1.19317(16) 0.0180(8) Uani 1 1 d . . .
C42 C 0.2565(2) 0.43711(14) 1.17913(16) 0.0164(8) Uani 1 1 d . . .
C43 C 0.3218(2) 0.45739(14) 1.22445(16) 0.0175(8) Uani 1 1 d . . .
C44 C 0.3916(2) 0.46842(16) 1.20601(18) 0.0232(9) Uani 1 1 d . . .
H44 H 0.3978 0.4620 1.1652 0.028 Uiso 1 1 calc R . .
C45 C 0.4516(2) 0.48897(18) 1.24853(19) 0.0309(10) Uani 1 1 d . . .
H45 H 0.4982 0.4955 1.2361 0.037 Uiso 1 1 calc R . .
C46 C 0.4431(3) 0.49978(17) 1.3083(2) 0.0353(11) Uani 1 1 d . . .
H46 H 0.4834 0.5147 1.3361 0.042 Uiso 1 1 calc R . .
C47 C 0.3748(3) 0.48858(18) 1.32745(19) 0.0339(10) Uani 1 1 d . . .
H47 H 0.3693 0.4952 1.3684 0.041 Uiso 1 1 calc R . .
C48 C 0.3142(2) 0.46750(16) 1.28587(17) 0.0247(9) Uani 1 1 d . . .
H48 H 0.2682 0.4601 1.2991 0.030 Uiso 1 1 calc R . .
C49 C 0.1542(2) 0.75521(16) 1.08740(18) 0.0225(8) Uani 1 1 d . . .
H49 H 0.1523 0.7357 1.1248 0.027 Uiso 1 1 calc R . .
C50 C 0.1721(2) 0.81639(16) 1.08753(19) 0.0289(10) Uani 1 1 d . . .
H50 H 0.1799 0.8383 1.1242 0.035 Uiso 1 1 calc R . .
C51 C 0.1784(3) 0.84441(17) 1.0325(2) 0.0371(11) Uani 1 1 d . . .
H51 H 0.1926 0.8852 1.0317 0.044 Uiso 1 1 calc R . .
C52 C 0.1632(2) 0.81137(16) 0.97795(19) 0.0290(10) Uani 1 1 d . . .
H52 H 0.1678 0.8298 0.9405 0.035 Uiso 1 1 calc R . .
C53 C 0.1412(2) 0.75058(15) 0.97965(17) 0.0190(8) Uani 1 1 d . . .
C54 C 0.11799(19) 0.71154(15) 0.92595(16) 0.0160(8) Uani 1 1 d . . .
C55 C 0.0960(2) 0.73522(15) 0.86274(17) 0.0193(8) Uani 1 1 d . . .
C56 C 0.1085(2) 0.70086(17) 0.81100(17) 0.0232(9) Uani 1 1 d . . .
H56 H 0.1299 0.6622 0.8163 0.028 Uiso 1 1 calc R . .
C57 C 0.0888(2) 0.72456(19) 0.75221(19) 0.0321(10) Uani 1 1 d . . .
H57 H 0.0968 0.7013 0.7184 0.039 Uiso 1 1 calc R . .
C58 C 0.0578(2) 0.78152(18) 0.7429(2) 0.0339(10) Uani 1 1 d . . .
H58 H 0.0460 0.7970 0.7031 0.041 Uiso 1 1 calc R . .
C59 C 0.0440(2) 0.81575(18) 0.7926(2) 0.0312(10) Uani 1 1 d . . .
H59 H 0.0227 0.8544 0.7862 0.037 Uiso 1 1 calc R . .
C60 C 0.0620(2) 0.79281(16) 0.85254(19) 0.0252(9) Uani 1 1 d . . .
H60 H 0.0514 0.8158 0.8858 0.030 Uiso 1 1 calc R . .
C61 C -0.0090(2) 0.54248(16) 0.78580(18) 0.0232(9) Uani 1 1 d . . .
H61 H 0.0311 0.5596 0.8122 0.028 Uiso 1 1 calc R . .
C62 C -0.0269(2) 0.56604(17) 0.72742(18) 0.0279(9) Uani 1 1 d . . .
H62 H -0.0005 0.5993 0.7152 0.034 Uiso 1 1 calc R . .
C63 C -0.0843(2) 0.53973(17) 0.68737(19) 0.0289(10) Uani 1 1 d . . .
H63 H -0.0960 0.5539 0.6471 0.035 Uiso 1 1 calc R . .
C64 C -0.1250(2) 0.49177(16) 0.70760(17) 0.0218(8) Uani 1 1 d . . .
H64 H -0.1644 0.4736 0.6813 0.026 Uiso 1 1 calc R . .
C65 C -0.1053(2) 0.47149(15) 0.76826(16) 0.0172(8) Uani 1 1 d . . .
C66 C -0.14936(19) 0.42523(14) 0.79692(16) 0.0150(8) Uani 1 1 d . . .
C67 C -0.2127(2) 0.39185(15) 0.75965(17) 0.0205(8) Uani 1 1 d . . .
C68 C -0.2839(2) 0.39209(15) 0.77770(18) 0.0213(8) Uani 1 1 d . . .
H68 H -0.2906 0.4100 0.8149 0.026 Uiso 1 1 calc R . .
C69 C -0.3441(2) 0.36595(17) 0.7407(2) 0.0327(10) Uani 1 1 d . . .
H69 H -0.3918 0.3671 0.7523 0.039 Uiso 1 1 calc R . .
C70 C -0.3336(3) 0.33763(19) 0.6858(2) 0.0420(12) Uani 1 1 d . . .
H70 H -0.3748 0.3212 0.6601 0.050 Uiso 1 1 calc R . .
C71 C -0.2633(3) 0.33390(18) 0.6696(2) 0.0388(11) Uani 1 1 d . . .
H71 H -0.2563 0.3128 0.6342 0.047 Uiso 1 1 calc R . .
C72 C -0.2020(2) 0.36152(17) 0.70577(18) 0.0283(9) Uani 1 1 d . . .
H72 H -0.1543 0.3598 0.6941 0.034 Uiso 1 1 calc R . .
C73 C 0.2455(3) 0.8378(2) 0.7910(3) 0.0611(15) Uani 1 1 d . . .
H73A H 0.2757 0.8535 0.8276 0.092 Uiso 1 1 calc R . .
H73B H 0.2778 0.8206 0.7645 0.092 Uiso 1 1 calc R . .
H73C H 0.2123 0.8068 0.8021 0.092 Uiso 1 1 calc R . .
C74 C 0.2016(3) 0.8867(3) 0.7591(2) 0.0488(13) Uani 1 1 d . . .
H74 H 0.195(3) 0.254(4) 1.030(3) 0.059 Uiso 0.50 1 d PD . .
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
Mn1 0.0112(3) 0.0174(3) 0.0148(3) -0.0022(2) 0.0026(2) -0.0002(2)
Mn2 0.0102(3) 0.0127(2) 0.0136(3) 0.0014(2) 0.0011(2) -0.0003(2)
Mn3 0.0099(3) 0.0182(3) 0.0175(3) 0.0025(2) 0.0000(2) 0.0010(2)
Mn4 0.0086(3) 0.0118(2) 0.0121(3) 0.0001(2) 0.0013(2) -0.0002(2)
Mn5 0.0094(3) 0.0118(2) 0.0146(3) 0.0006(2) 0.0006(2) -0.0002(2)
Mn6 0.0101(3) 0.0143(3) 0.0125(3) -0.0012(2) 0.0012(2) -0.0007(2)
Cl1 0.0934(12) 0.0491(8) 0.0477(8) 0.0166(6) 0.0242(8) 0.0041(8)
Cl2 0.080(2) 0.114(3) 0.0592(19) 0.022(2) 0.0270(19) -0.001(2)
N1 0.0156(17) 0.0326(17) 0.0161(17) -0.0008(14) 0.0034(14) 0.0037(14)
N2 0.0130(16) 0.0200(15) 0.0144(16) -0.0006(13) 0.0017(13) 0.0013(12)
N3 0.0143(17) 0.0247(16) 0.0236(18) -0.0034(13) 0.0035(14) -0.0010(13)
N4 0.0144(16) 0.0231(16) 0.0177(16) -0.0050(13) 0.0028(13) 0.0000(13)
N5 0.0130(16) 0.0191(15) 0.0173(16) 0.0006(12) 0.0018(13) 0.0011(13)
N6 0.0110(16) 0.0165(14) 0.0160(16) 0.0012(12) 0.0048(13) 0.0011(12)
N7 0.0136(16) 0.0214(15) 0.0223(17) 0.0022(13) 0.0045(14) -0.0002(13)
N8 0.0131(16) 0.0132(14) 0.0177(16) 0.0041(12) 0.0028(13) -0.0010(12)
N9 0.0112(16) 0.0131(14) 0.0220(17) -0.0002(12) 0.0010(13) 0.0019(12)
N10 0.0114(15) 0.0163(14) 0.0145(15) 0.0008(12) 0.0033(13) -0.0012(12)
N11 0.0164(16) 0.0168(14) 0.0165(16) -0.0018(12) 0.0052(14) -0.0006(13)
N12 0.0119(16) 0.0140(14) 0.0172(16) 0.0004(12) 0.0025(13) 0.0004(12)
N13 0.057(3) 0.079(3) 0.081(4) 0.028(3) 0.003(3) -0.028(3)
O1 0.0120(13) 0.0236(13) 0.0180(13) 0.0013(10) -0.0001(11) -0.0028(10)
O2 0.0099(13) 0.0188(12) 0.0202(13) -0.0065(10) 0.0005(11) -0.0003(10)
O3 0.0111(13) 0.0142(11) 0.0223(14) 0.0016(10) 0.0007(11) 0.0000(10)
O4 0.0167(13) 0.0127(11) 0.0155(13) 0.0027(10) -0.0012(11) -0.0032(10)
O5 0.0178(13) 0.0162(12) 0.0145(13) 0.0019(10) 0.0002(11) -0.0035(10)
O6 0.0133(13) 0.0171(12) 0.0146(13) 0.0010(10) 0.0007(10) -0.0027(10)
O7 0.0132(13) 0.0148(11) 0.0159(13) 0.0004(10) 0.0000(10) -0.0006(10)
O8 0.0110(13) 0.0162(12) 0.0182(13) -0.0040(10) 0.0020(11) -0.0018(10)
O9 0.0084(12) 0.0116(11) 0.0194(13) 0.0004(10) 0.0014(10) -0.0014(9)
O10 0.0111(12) 0.0149(11) 0.0136(12) -0.0001(9) 0.0012(10) -0.0011(10)
O11 0.0102(12) 0.0120(11) 0.0133(12) 0.0018(9) -0.0004(10) 0.0004(9)
O12 0.0248(15) 0.0227(13) 0.0313(16) 0.0021(11) -0.0008(13) 0.0004(11)
O13A 0.079(5) 0.028(3) 0.069(4) -0.006(2) 0.022(3) -0.004(3)
O13B 0.084(6) 0.054(5) 0.109(7) 0.009(4) -0.001(5) 0.008(4)
O14A 0.082(7) 0.066(7) 0.092(8) -0.008(4) -0.002(5) 0.027(4)
O14B 0.061(5) 0.043(4) 0.037(4) -0.006(3) 0.027(3) 0.013(3)
O14C 0.042(6) 0.043(6) 0.023(6) -0.007(4) 0.000(4) 0.008(4)
O15 0.060(3) 0.0443(19) 0.071(3) 0.0133(18) 0.002(2) 0.0040(18)
O16A 0.087(4) 0.111(5) 0.106(5) 0.015(3) 0.000(3) 0.043(3)
O16B 0.077(8) 0.089(8) 0.091(8) 0.004(5) 0.026(5) 0.006(4)
O17 0.102(3) 0.119(3) 0.074(3) -0.015(3) 0.014(3) 0.005(3)
O18 0.110(5) 0.138(5) 0.098(5) 0.012(4) 0.014(4) 0.010(4)
O19 0.148(6) 0.135(6) 0.141(6) 0.022(4) 0.027(5) 0.014(4)
O20 0.031(4) 0.021(3) 0.068(5) -0.013(3) -0.015(3) 0.021(3)
C1 0.022(2) 0.045(2) 0.021(2) -0.0123(19) 0.0037(18) 0.0030(19)
C2 0.031(3) 0.065(3) 0.019(2) -0.006(2) -0.002(2) 0.005(2)
C3 0.035(3) 0.075(3) 0.017(2) 0.009(2) 0.003(2) 0.017(3)
C4 0.023(2) 0.048(3) 0.029(2) 0.013(2) 0.009(2) 0.006(2)
C5 0.017(2) 0.032(2) 0.0158(19) 0.0017(16) 0.0076(17) 0.0066(17)
C6 0.0124(19) 0.0272(19) 0.018(2) 0.0043(16) 0.0067(16) 0.0094(16)
C7 0.015(2) 0.032(2) 0.022(2) 0.0134(17) 0.0041(17) 0.0032(17)
C8 0.022(2) 0.043(2) 0.027(2) 0.0136(19) 0.0086(19) 0.0042(19)
C9 0.024(2) 0.064(3) 0.041(3) 0.026(3) 0.013(2) 0.000(2)
C10 0.036(3) 0.046(3) 0.054(3) 0.020(3) 0.007(3) -0.012(2)
C11 0.044(3) 0.033(2) 0.044(3) 0.012(2) 0.001(2) -0.008(2)
C12 0.024(2) 0.030(2) 0.031(2) 0.0126(18) 0.0070(19) 0.0009(18)
C13 0.014(2) 0.032(2) 0.033(2) -0.0082(18) 0.0015(18) -0.0024(17)
C14 0.018(2) 0.038(2) 0.052(3) -0.009(2) 0.007(2) 0.0075(19)
C15 0.031(3) 0.029(2) 0.059(3) -0.012(2) 0.014(2) 0.0068(19)
C16 0.024(2) 0.025(2) 0.046(3) -0.0103(19) 0.010(2) -0.0007(18)
C17 0.020(2) 0.0241(19) 0.024(2) -0.0046(16) 0.0050(17) 0.0028(16)
C18 0.017(2) 0.0242(19) 0.020(2) -0.0074(16) 0.0042(17) -0.0046(16)
C19 0.014(2) 0.026(2) 0.034(2) -0.0164(17) 0.0097(18) -0.0010(16)
C20 0.036(3) 0.026(2) 0.049(3) -0.013(2) 0.018(2) -0.0079(19)
C21 0.032(3) 0.038(3) 0.077(4) -0.024(3) 0.022(3) -0.013(2)
C22 0.029(3) 0.030(3) 0.107(5) -0.046(3) 0.028(3) -0.011(2)
C23 0.023(3) 0.057(3) 0.071(4) -0.047(3) -0.008(2) 0.008(2)
C24 0.024(2) 0.030(2) 0.053(3) -0.019(2) -0.005(2) 0.0036(19)
C25 0.020(2) 0.0230(19) 0.018(2) 0.0005(15) 0.0037(17) 0.0020(16)
C26 0.015(2) 0.0247(19) 0.027(2) 0.0025(16) 0.0036(17) 0.0056(16)
C27 0.013(2) 0.038(2) 0.022(2) 0.0030(17) -0.0007(17) 0.0010(17)
C28 0.0111(19) 0.0246(19) 0.022(2) -0.0017(16) 0.0018(16) -0.0008(15)
C29 0.0123(19) 0.0221(18) 0.019(2) 0.0018(15) 0.0050(16) -0.0013(15)
C30 0.0129(19) 0.0207(18) 0.0165(19) 0.0006(15) 0.0021(16) -0.0027(15)
C31 0.0139(19) 0.0188(18) 0.024(2) -0.0007(16) -0.0026(16) -0.0028(15)
C32 0.031(2) 0.027(2) 0.039(3) -0.0076(19) 0.014(2) -0.0064(18)
C33 0.050(3) 0.027(2) 0.059(3) -0.018(2) 0.015(3) -0.011(2)
C34 0.045(3) 0.025(2) 0.056(3) -0.005(2) 0.000(3) -0.015(2)
C35 0.029(3) 0.034(2) 0.041(3) 0.006(2) 0.002(2) -0.016(2)
C36 0.020(2) 0.027(2) 0.029(2) 0.0018(17) 0.0009(18) -0.0038(17)
C37 0.014(2) 0.0232(19) 0.032(2) 0.0016(17) 0.0046(18) -0.0016(16)
C38 0.023(2) 0.026(2) 0.041(3) 0.0086(19) 0.010(2) -0.0012(18)
C39 0.037(3) 0.029(2) 0.028(2) 0.0151(18) 0.003(2) 0.0011(19)
C40 0.023(2) 0.027(2) 0.024(2) 0.0072(17) -0.0001(18) -0.0006(17)
C41 0.015(2) 0.0208(18) 0.0188(19) 0.0015(15) 0.0048(17) 0.0041(15)
C42 0.0159(19) 0.0136(16) 0.019(2) 0.0012(14) 0.0020(16) 0.0063(14)
C43 0.018(2) 0.0123(16) 0.020(2) 0.0040(14) -0.0048(16) 0.0028(15)
C44 0.023(2) 0.0230(19) 0.023(2) 0.0089(16) 0.0005(18) 0.0010(16)
C45 0.020(2) 0.035(2) 0.034(3) 0.0085(19) -0.0081(19) -0.0036(18)
C46 0.033(3) 0.029(2) 0.037(3) 0.0043(19) -0.019(2) -0.0020(19)
C47 0.048(3) 0.031(2) 0.019(2) -0.0005(18) -0.009(2) 0.011(2)
C48 0.025(2) 0.025(2) 0.022(2) 0.0050(16) -0.0023(18) 0.0077(17)
C49 0.021(2) 0.0235(19) 0.023(2) -0.0006(16) 0.0035(17) 0.0007(16)
C50 0.039(3) 0.0180(19) 0.029(2) -0.0079(17) 0.002(2) -0.0023(17)
C51 0.052(3) 0.0176(19) 0.040(3) -0.0036(19) 0.001(2) -0.0095(19)
C52 0.040(3) 0.0165(18) 0.030(2) 0.0014(17) 0.004(2) -0.0077(18)
C53 0.015(2) 0.0158(17) 0.025(2) 0.0041(15) 0.0010(17) 0.0010(15)
C54 0.0123(18) 0.0145(17) 0.021(2) 0.0044(15) 0.0030(16) 0.0008(14)
C55 0.0106(19) 0.0176(18) 0.029(2) 0.0076(16) 0.0009(16) -0.0035(15)
C56 0.020(2) 0.0238(19) 0.026(2) 0.0063(17) 0.0047(18) -0.0027(17)
C57 0.033(2) 0.042(2) 0.022(2) 0.0067(19) 0.008(2) -0.006(2)
C58 0.029(2) 0.039(2) 0.032(2) 0.022(2) -0.003(2) -0.009(2)
C59 0.020(2) 0.027(2) 0.045(3) 0.019(2) -0.002(2) -0.0045(17)
C60 0.022(2) 0.0208(19) 0.033(2) 0.0042(17) 0.0044(19) -0.0028(16)
C61 0.024(2) 0.0216(19) 0.026(2) -0.0018(16) 0.0104(18) -0.0013(17)
C62 0.037(3) 0.0223(19) 0.028(2) 0.0075(17) 0.013(2) -0.0037(18)
C63 0.036(3) 0.030(2) 0.022(2) 0.0066(18) 0.010(2) 0.0050(19)
C64 0.023(2) 0.0272(19) 0.0153(19) 0.0013(16) 0.0016(17) 0.0060(17)
C65 0.016(2) 0.0180(17) 0.0175(19) 0.0013(15) 0.0026(16) 0.0066(15)
C66 0.0127(19) 0.0163(17) 0.0152(19) 0.0015(14) -0.0001(16) 0.0036(14)
C67 0.025(2) 0.0151(17) 0.019(2) 0.0009(15) -0.0041(17) -0.0006(16)
C68 0.020(2) 0.0153(17) 0.026(2) 0.0025(16) -0.0040(17) 0.0000(16)
C69 0.024(2) 0.028(2) 0.042(3) 0.0043(19) -0.009(2) -0.0031(18)
C70 0.047(3) 0.035(2) 0.035(3) 0.002(2) -0.021(2) -0.015(2)
C71 0.056(3) 0.030(2) 0.025(2) -0.0134(18) -0.010(2) -0.005(2)
C72 0.033(2) 0.029(2) 0.021(2) -0.0026(17) -0.0005(19) 0.0069(18)
C73 0.048(3) 0.069(4) 0.064(4) 0.010(3) 0.002(3) -0.029(3)
C74 0.043(3) 0.066(3) 0.037(3) 0.004(3) 0.007(3) -0.032(3)
_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
Mn1 O8 2.042(2) . ?
Mn1 N2 2.210(3) . ?
Mn1 N4 2.229(3) . ?
Mn1 N3 2.248(3) . ?
Mn1 O7 2.249(2) . ?
Mn1 N1 2.353(3) . ?
Mn2 O1 1.881(2) . ?
Mn2 O4 1.902(2) . ?
Mn2 O7 1.983(2) . ?
Mn2 O9 2.080(2) . ?
Mn2 N6 2.119(3) . ?
Mn2 N5 2.268(3) . ?
Mn3 O11 2.038(2) . ?
Mn3 O12 2.107(3) . ?
Mn3 N8 2.195(3) . ?
Mn3 O7 2.250(2) . ?
Mn3 N7 2.265(3) . ?
Mn4 O8 1.851(2) . ?
Mn4 O9 1.932(2) . ?
Mn4 O11 1.939(2) 3_567 ?
Mn4 O10 1.941(2) . ?
Mn4 O5 2.291(2) . ?
Mn4 O11 2.294(2) . ?
Mn4 Mn5 2.7300(7) . ?
Mn4 Mn6 2.8205(7) . ?
Mn4 Mn6 3.0800(7) 3_567 ?
Mn4 Mn4 3.1561(9) 3_567 ?
Mn5 O9 1.810(2) . ?
Mn5 O10 1.838(2) . ?
Mn5 O6 1.893(2) 3_567 ?
Mn5 O3 1.960(2) . ?
Mn5 N10 2.007(3) . ?
Mn5 N9 2.060(3) . ?
Mn6 O8 1.847(2) . ?
Mn6 O11 1.928(2) 3_567 ?
Mn6 O2 1.930(2) . ?
Mn6 N12 2.107(3) . ?
Mn6 O10 2.161(2) 3_567 ?
Mn6 N11 2.247(3) . ?
Mn6 Mn4 3.0801(7) 3_567 ?
Cl1 O13B 1.200(10) . ?
Cl1 O14B 1.351(6) . ?
Cl1 O15 1.402(3) . ?
Cl1 O13A 1.479(7) . ?
Cl1 O16A 1.530(7) . ?
Cl1 O14A 1.536(15) . ?
Cl1 O16B 1.539(14) . ?
Cl1 O14C 1.602(12) . ?
Cl2 O17 1.342(5) . ?
Cl2 O19 1.425(12) . ?
Cl2 O18 1.471(11) . ?
Cl2 O17 1.507(6) 3_566 ?
Cl2 Cl2 1.581(7) 3_566 ?
N1 C1 1.342(5) . ?
N1 C5 1.357(5) . ?
N2 C6 1.301(4) . ?
N2 O1 1.358(4) . ?
N3 C13 1.328(5) . ?
N3 C17 1.362(5) . ?
N4 C18 1.284(4) . ?
N4 O2 1.351(4) . ?
N5 C25 1.335(4) . ?
N5 C29 1.347(4) . ?
N6 C30 1.300(4) . ?
N6 O3 1.355(3) . ?
N7 C37 1.339(4) . ?
N7 C41 1.348(5) . ?
N8 C42 1.299(4) . ?
N8 O4 1.356(3) . ?
N9 C49 1.338(5) . ?
N9 C53 1.364(4) . ?
N10 C54 1.310(4) . ?
N10 O5 1.311(3) . ?
N11 C61 1.332(4) . ?
N11 C65 1.355(5) . ?
N12 C66 1.292(4) . ?
N12 O6 1.362(3) . ?
N13 C74 1.143(7) . ?
O6 Mn5 1.894(2) 3_567 ?
O10 Mn6 2.161(2) 3_567 ?
O11 Mn6 1.928(2) 3_567 ?
O11 Mn4 1.939(2) 3_567 ?
O13A O13B 1.115(13) . ?
O13B O16A 1.426(15) . ?
O14A O14B 1.310(17) . ?
O14B O14C 1.198(14) . ?
O15 O16B 1.329(16) . ?
O16A O16B 1.421(16) . ?
O17 Cl2 1.507(6) 3_566 ?
O20 H74 0.92(2) . ?
C1 C2 1.385(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.367(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.397(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.469(5) . ?
C6 C7 1.485(5) . ?
C7 C12 1.385(5) . ?
C7 C8 1.398(5) . ?
C8 C9 1.397(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.367(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.378(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.488(5) . ?
C18 C19 1.496(5) . ?
C19 C24 1.369(6) . ?
C19 C20 1.387(6) . ?
C20 C21 1.376(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.348(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.371(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.407(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.370(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.389(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.485(5) . ?
C30 C31 1.487(5) . ?
C31 C32 1.385(5) . ?
C31 C36 1.386(5) . ?
C32 C33 1.391(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.378(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.394(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C38 1.380(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.381(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.382(5) . ?
C39 H39 0.9300 . ?
C40 C41 1.389(5) . ?
C40 H40 0.9300 . ?
C41 C42 1.493(5) . ?
C42 C43 1.483(5) . ?
C43 C48 1.393(5) . ?
C43 C44 1.395(5) . ?
C44 C45 1.387(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.364(6) . ?
C45 H45 0.9300 . ?
C46 C47 1.379(6) . ?
C46 H46 0.9300 . ?
C47 C48 1.387(6) . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 C50 1.379(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.375(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.388(6) . ?
C51 H51 0.9300 . ?
C52 C53 1.392(5) . ?
C52 H52 0.9300 . ?
C53 C54 1.464(5) . ?
C54 C55 1.476(5) . ?
C55 C60 1.405(5) . ?
C55 C56 1.409(5) . ?
C56 C57 1.385(5) . ?
C56 H56 0.9300 . ?
C57 C58 1.369(6) . ?
C57 H57 0.9300 . ?
C58 C59 1.376(6) . ?
C58 H58 0.9300 . ?
C59 C60 1.399(6) . ?
C59 H59 0.9300 . ?
C60 H60 0.9300 . ?
C61 C62 1.372(5) . ?
C61 H61 0.9300 . ?
C62 C63 1.374(6) . ?
C62 H62 0.9300 . ?
C63 C64 1.391(5) . ?
C63 H63 0.9300 . ?
C64 C65 1.396(5) . ?
C64 H64 0.9300 . ?
C65 C66 1.484(5) . ?
C66 C67 1.486(5) . ?
C67 C72 1.395(5) . ?
C67 C68 1.396(5) . ?
C68 C69 1.371(5) . ?
C68 H68 0.9300 . ?
C69 C70 1.393(6) . ?
C69 H69 0.9300 . ?
C70 C71 1.367(6) . ?
C70 H70 0.9300 . ?
C71 C72 1.391(6) . ?
C71 H71 0.9300 . ?
C72 H72 0.9300 . ?
C73 C74 1.446(8) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
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
O8 Mn1 N2 102.27(9) . . ?
O8 Mn1 N4 78.59(10) . . ?
N2 Mn1 N4 156.02(11) . . ?
O8 Mn1 N3 144.98(10) . . ?
N2 Mn1 N3 112.45(10) . . ?
N4 Mn1 N3 71.65(11) . . ?
O8 Mn1 O7 88.04(9) . . ?
N2 Mn1 O7 81.92(9) . . ?
N4 Mn1 O7 121.98(9) . . ?
N3 Mn1 O7 92.26(10) . . ?
O8 Mn1 N1 99.79(10) . . ?
N2 Mn1 N1 70.02(11) . . ?
N4 Mn1 N1 86.15(11) . . ?
N3 Mn1 N1 96.28(11) . . ?
O7 Mn1 N1 151.85(10) . . ?
O1 Mn2 O4 164.53(11) . . ?
O1 Mn2 O7 93.50(10) . . ?
O4 Mn2 O7 94.52(9) . . ?
O1 Mn2 O9 97.81(10) . . ?
O4 Mn2 O9 95.84(10) . . ?
O7 Mn2 O9 86.67(9) . . ?
O1 Mn2 N6 87.38(10) . . ?
O4 Mn2 N6 87.02(10) . . ?
O7 Mn2 N6 169.94(10) . . ?
O9 Mn2 N6 83.29(10) . . ?
O1 Mn2 N5 83.74(10) . . ?
O4 Mn2 N5 80.86(10) . . ?
O7 Mn2 N5 116.11(10) . . ?
O9 Mn2 N5 157.11(9) . . ?
N6 Mn2 N5 73.95(10) . . ?
O11 Mn3 O12 99.03(10) . . ?
O11 Mn3 N8 115.05(10) . . ?
O12 Mn3 N8 143.63(10) . . ?
O11 Mn3 O7 124.53(8) . . ?
O12 Mn3 O7 93.89(9) . . ?
N8 Mn3 O7 77.60(9) . . ?
O11 Mn3 N7 103.07(9) . . ?
O12 Mn3 N7 90.16(10) . . ?
N8 Mn3 N7 70.79(10) . . ?
O7 Mn3 N7 130.73(10) . . ?
O8 Mn4 O9 96.99(10) . . ?
O8 Mn4 O11 83.23(9) . 3_567 ?
O9 Mn4 O11 172.91(9) . 3_567 ?
O8 Mn4 O10 174.65(10) . . ?
O9 Mn4 O10 79.70(9) . . ?
O11 Mn4 O10 99.54(9) 3_567 . ?
O8 Mn4 O5 97.98(9) . . ?
O9 Mn4 O5 82.97(9) . . ?
O11 Mn4 O5 104.04(9) 3_567 . ?
O10 Mn4 O5 85.83(9) . . ?
O8 Mn4 O11 93.33(9) . . ?
O9 Mn4 O11 88.96(9) . . ?
O11 Mn4 O11 83.96(9) 3_567 . ?
O10 Mn4 O11 82.47(8) . . ?
O5 Mn4 O11 166.82(8) . . ?
O8 Mn4 Mn5 135.94(7) . . ?
O9 Mn4 Mn5 41.43(6) . . ?
O11 Mn4 Mn5 140.03(6) 3_567 . ?
O10 Mn4 Mn5 42.26(7) . . ?
O5 Mn4 Mn5 68.70(6) . . ?
O11 Mn4 Mn5 98.40(6) . . ?
O8 Mn4 Mn6 40.23(7) . . ?
O9 Mn4 Mn6 136.75(7) . . ?
O11 Mn4 Mn6 43.00(6) 3_567 . ?
O10 Mn4 Mn6 142.30(7) . . ?
O5 Mn4 Mn6 104.92(6) . . ?
O11 Mn4 Mn6 88.10(6) . . ?
Mn5 Mn4 Mn6 172.97(2) . . ?
O8 Mn4 Mn6 131.92(7) . 3_567 ?
O9 Mn4 Mn6 86.80(7) . 3_567 ?
O11 Mn4 Mn6 87.81(7) 3_567 3_567 ?
O10 Mn4 Mn6 44.12(6) . 3_567 ?
O5 Mn4 Mn6 129.95(6) . 3_567 ?
O11 Mn4 Mn6 38.67(5) . 3_567 ?
Mn5 Mn4 Mn6 71.487(18) . 3_567 ?
Mn6 Mn4 Mn6 115.504(18) . 3_567 ?
O8 Mn4 Mn4 88.27(7) . 3_567 ?
O9 Mn4 Mn4 126.62(7) . 3_567 ?
O11 Mn4 Mn4 46.29(6) 3_567 3_567 ?
O10 Mn4 Mn4 90.37(7) . 3_567 ?
O5 Mn4 Mn4 148.96(7) . 3_567 ?
O11 Mn4 Mn4 37.66(6) . 3_567 ?
Mn5 Mn4 Mn4 125.24(3) . 3_567 ?
Mn6 Mn4 Mn4 61.741(18) . 3_567 ?
Mn6 Mn4 Mn4 53.763(17) 3_567 3_567 ?
O9 Mn5 O10 85.73(10) . . ?
O9 Mn5 O6 100.28(10) . 3_567 ?
O10 Mn5 O6 94.37(10) . 3_567 ?
O9 Mn5 O3 92.37(9) . . ?
O10 Mn5 O3 176.38(10) . . ?
O6 Mn5 O3 89.00(10) 3_567 . ?
O9 Mn5 N10 91.23(11) . . ?
O10 Mn5 N10 84.56(11) . . ?
O6 Mn5 N10 168.34(10) 3_567 . ?
O3 Mn5 N10 92.41(10) . . ?
O9 Mn5 N9 165.35(11) . . ?
O10 Mn5 N9 102.08(10) . . ?
O6 Mn5 N9 91.54(11) 3_567 . ?
O3 Mn5 N9 79.12(10) . . ?
N10 Mn5 N9 77.38(11) . . ?
O9 Mn5 Mn4 44.92(7) . . ?
O10 Mn5 Mn4 45.27(7) . . ?
O6 Mn5 Mn4 115.57(7) 3_567 . ?
O3 Mn5 Mn4 131.77(7) . . ?
N10 Mn5 Mn4 71.61(8) . . ?
N9 Mn5 Mn4 135.88(9) . . ?
O8 Mn6 O11 83.66(9) . 3_567 ?
O8 Mn6 O2 92.97(10) . . ?
O11 Mn6 O2 174.99(10) 3_567 . ?
O8 Mn6 N12 172.67(10) . . ?
O11 Mn6 N12 102.24(10) 3_567 . ?
O2 Mn6 N12 81.41(10) . . ?
O8 Mn6 O10 101.91(9) . 3_567 ?
O11 Mn6 O10 86.41(8) 3_567 3_567 ?
O2 Mn6 O10 90.68(9) . 3_567 ?
N12 Mn6 O10 82.96(10) . 3_567 ?
O8 Mn6 N11 102.21(10) . . ?
O11 Mn6 N11 93.59(9) 3_567 . ?
O2 Mn6 N11 90.74(10) . . ?
N12 Mn6 N11 73.31(11) . . ?
O10 Mn6 N11 155.73(10) 3_567 . ?
O8 Mn6 Mn4 40.34(7) . . ?
O11 Mn6 Mn4 43.32(7) 3_567 . ?
O2 Mn6 Mn4 133.19(7) . . ?
N12 Mn6 Mn4 145.39(7) . . ?
O10 Mn6 Mn4 95.57(6) 3_567 . ?
N11 Mn6 Mn4 101.03(7) . . ?
O8 Mn6 Mn4 90.69(7) . 3_567 ?
O11 Mn6 Mn4 48.04(6) 3_567 3_567 ?
O2 Mn6 Mn4 128.55(7) . 3_567 ?
N12 Mn6 Mn4 96.49(8) . 3_567 ?
O10 Mn6 Mn4 38.71(6) 3_567 3_567 ?
N11 Mn6 Mn4 138.19(7) . 3_567 ?
Mn4 Mn6 Mn4 64.496(18) . 3_567 ?
O13B Cl1 O14B 101.4(7) . . ?
O13B Cl1 O15 140.7(7) . . ?
O14B Cl1 O15 117.7(3) . . ?
O13B Cl1 O13A 47.8(7) . . ?
O14B Cl1 O13A 114.0(4) . . ?
O15 Cl1 O13A 107.5(3) . . ?
O13B Cl1 O16A 61.6(7) . . ?
O14B Cl1 O16A 107.4(5) . . ?
O15 Cl1 O16A 106.9(4) . . ?
O13A Cl1 O16A 102.1(4) . . ?
O13B Cl1 O14A 113.9(9) . . ?
O14B Cl1 O14A 53.5(6) . . ?
O15 Cl1 O14A 88.3(6) . . ?
O13A Cl1 O14A 84.5(6) . . ?
O16A Cl1 O14A 160.4(7) . . ?
O13B Cl1 O16B 98.1(8) . . ?
O14B Cl1 O16B 141.4(7) . . ?
O15 Cl1 O16B 53.5(6) . . ?
O13A Cl1 O16B 103.8(6) . . ?
O16A Cl1 O16B 55.2(6) . . ?
O14A Cl1 O16B 141.7(9) . . ?
O13B Cl1 O14C 116.6(9) . . ?
O14B Cl1 O14C 46.9(5) . . ?
O15 Cl1 O14C 94.5(5) . . ?
O13A Cl1 O14C 157.0(5) . . ?
O16A Cl1 O14C 77.1(5) . . ?
O14A Cl1 O14C 89.6(8) . . ?
O16B Cl1 O14C 94.6(8) . . ?
O17 Cl2 O19 108.7(6) . . ?
O17 Cl2 O18 114.3(5) . . ?
O19 Cl2 O18 116.9(7) . . ?
O17 Cl2 O17 112.9(3) . 3_566 ?
O19 Cl2 O17 99.6(6) . 3_566 ?
O18 Cl2 O17 103.5(5) . 3_566 ?
O17 Cl2 Cl2 61.4(3) . 3_566 ?
O19 Cl2 Cl2 115.5(7) . 3_566 ?
O18 Cl2 Cl2 124.8(6) . 3_566 ?
O17 Cl2 Cl2 51.5(3) 3_566 3_566 ?
C1 N1 C5 118.0(3) . . ?
C1 N1 Mn1 126.6(3) . . ?
C5 N1 Mn1 115.1(2) . . ?
C6 N2 O1 115.1(3) . . ?
C6 N2 Mn1 123.3(2) . . ?
O1 N2 Mn1 121.4(2) . . ?
C13 N3 C17 117.7(3) . . ?
C13 N3 Mn1 125.6(2) . . ?
C17 N3 Mn1 116.7(2) . . ?
C18 N4 O2 116.5(3) . . ?
C18 N4 Mn1 121.0(2) . . ?
O2 N4 Mn1 122.52(19) . . ?
C25 N5 C29 118.7(3) . . ?
C25 N5 Mn2 127.2(2) . . ?
C29 N5 Mn2 112.9(2) . . ?
C30 N6 O3 118.3(3) . . ?
C30 N6 Mn2 120.7(2) . . ?
O3 N6 Mn2 120.1(2) . . ?
C37 N7 C41 118.6(3) . . ?
C37 N7 Mn3 123.9(3) . . ?
C41 N7 Mn3 116.1(2) . . ?
C42 N8 O4 117.0(3) . . ?
C42 N8 Mn3 123.4(2) . . ?
O4 N8 Mn3 119.6(2) . . ?
C49 N9 C53 120.1(3) . . ?
C49 N9 Mn5 124.8(2) . . ?
C53 N9 Mn5 112.1(2) . . ?
C54 N10 O5 123.4(3) . . ?
C54 N10 Mn5 119.0(2) . . ?
O5 N10 Mn5 117.26(19) . . ?
C61 N11 C65 118.8(3) . . ?
C61 N11 Mn6 128.3(3) . . ?
C65 N11 Mn6 112.8(2) . . ?
C66 N12 O6 115.9(3) . . ?
C66 N12 Mn6 119.6(2) . . ?
O6 N12 Mn6 121.3(2) . . ?
N2 O1 Mn2 118.33(18) . . ?
N4 O2 Mn6 116.55(19) . . ?
N6 O3 Mn5 115.97(17) . . ?
N8 O4 Mn2 115.64(19) . . ?
N10 O5 Mn4 100.13(17) . . ?
N12 O6 Mn5 117.33(19) . 3_567 ?
Mn2 O7 Mn1 112.55(10) . . ?
Mn2 O7 Mn3 104.04(9) . . ?
Mn1 O7 Mn3 109.92(10) . . ?
Mn6 O8 Mn4 99.42(10) . . ?
Mn6 O8 Mn1 125.76(11) . . ?
Mn4 O8 Mn1 134.47(12) . . ?
Mn5 O9 Mn4 93.65(10) . . ?
Mn5 O9 Mn2 120.72(11) . . ?
Mn4 O9 Mn2 145.33(12) . . ?
Mn5 O10 Mn4 92.47(9) . . ?
Mn5 O10 Mn6 116.56(11) . 3_567 ?
Mn4 O10 Mn6 97.17(9) . 3_567 ?
Mn6 O11 Mn4 93.67(9) 3_567 3_567 ?
Mn6 O11 Mn3 133.07(12) 3_567 . ?
Mn4 O11 Mn3 129.36(11) 3_567 . ?
Mn6 O11 Mn4 93.29(8) 3_567 . ?
Mn4 O11 Mn4 96.05(9) 3_567 . ?
Mn3 O11 Mn4 98.80(9) . . ?
O13B O13A Cl1 52.8(6) . . ?
O13A O13B Cl1 79.4(9) . . ?
O13A O13B O16A 133.7(12) . . ?
Cl1 O13B O16A 70.7(7) . . ?
O14B O14A Cl1 56.0(7) . . ?
O14C O14B O14A 123.6(11) . . ?
O14C O14B Cl1 77.6(6) . . ?
O14A O14B Cl1 70.5(7) . . ?
O14B O14C Cl1 55.4(6) . . ?
O16B O15 Cl1 68.5(7) . . ?
O16B O16A O13B 93.9(10) . . ?
O16B O16A Cl1 62.7(7) . . ?
O13B O16A Cl1 47.7(5) . . ?
O15 O16B O16A 117.9(11) . . ?
O15 O16B Cl1 58.0(6) . . ?
O16A O16B Cl1 62.1(7) . . ?
Cl2 O17 Cl2 67.1(3) . 3_566 ?
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.5(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 116.1(3) . . ?
C4 C5 C6 122.4(4) . . ?
N2 C6 C5 115.0(3) . . ?
N2 C6 C7 122.7(3) . . ?
C5 C6 C7 122.2(3) . . ?
C12 C7 C8 119.1(4) . . ?
C12 C7 C6 120.4(3) . . ?
C8 C7 C6 120.5(3) . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C10 C9 C8 121.2(4) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C7 C12 C11 120.8(4) . . ?
C7 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
N3 C13 C14 124.1(4) . . ?
N3 C13 H13 117.9 . . ?
C14 C13 H13 117.9 . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C17 118.8(4) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
N3 C17 C16 121.7(3) . . ?
N3 C17 C18 115.8(3) . . ?
C16 C17 C18 122.5(3) . . ?
N4 C18 C17 114.8(3) . . ?
N4 C18 C19 123.8(3) . . ?
C17 C18 C19 121.4(3) . . ?
C24 C19 C20 119.6(4) . . ?
C24 C19 C18 120.0(4) . . ?
C20 C19 C18 120.4(4) . . ?
C21 C20 C19 120.5(5) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 119.7(5) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.4(4) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C24 119.2(5) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C19 C24 C23 119.4(5) . . ?
C19 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
N5 C25 C26 123.2(3) . . ?
N5 C25 H25 118.4 . . ?
C26 C25 H25 118.4 . . ?
C25 C26 C27 118.6(3) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
C28 C27 C26 118.7(4) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C27 C28 C29 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
N5 C29 C28 120.9(3) . . ?
N5 C29 C30 116.1(3) . . ?
C28 C29 C30 123.0(3) . . ?
N6 C30 C29 114.9(3) . . ?
N6 C30 C31 123.9(3) . . ?
C29 C30 C31 121.2(3) . . ?
C32 C31 C36 119.0(3) . . ?
C32 C31 C30 121.3(3) . . ?
C36 C31 C30 119.7(3) . . ?
C31 C32 C33 120.4(4) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 120.3(4) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C35 C34 C33 119.7(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.4(4) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 120.3(4) . . ?
C31 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
N7 C37 C38 122.9(4) . . ?
N7 C37 H37 118.6 . . ?
C38 C37 H37 118.6 . . ?
C37 C38 C39 118.3(4) . . ?
C37 C38 H38 120.8 . . ?
C39 C38 H38 120.8 . . ?
C38 C39 C40 119.5(4) . . ?
C38 C39 H39 120.2 . . ?
C40 C39 H39 120.2 . . ?
C39 C40 C41 118.9(4) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
N7 C41 C40 121.5(3) . . ?
N7 C41 C42 116.0(3) . . ?
C40 C41 C42 122.4(3) . . ?
N8 C42 C43 125.9(3) . . ?
N8 C42 C41 112.2(3) . . ?
C43 C42 C41 121.9(3) . . ?
C48 C43 C44 118.7(3) . . ?
C48 C43 C42 120.7(3) . . ?
C44 C43 C42 120.6(3) . . ?
C45 C44 C43 120.0(4) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C46 C45 C44 120.8(4) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 119.9(4) . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C46 C47 C48 120.2(4) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C47 C48 C43 120.3(4) . . ?
C47 C48 H48 119.8 . . ?
C43 C48 H48 119.8 . . ?
N9 C49 C50 122.0(3) . . ?
N9 C49 H49 119.0 . . ?
C50 C49 H49 119.0 . . ?
C51 C50 C49 118.9(4) . . ?
C51 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C50 C51 C52 119.5(4) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
C51 C52 C53 119.7(4) . . ?
C51 C52 H52 120.2 . . ?
C53 C52 H52 120.2 . . ?
N9 C53 C52 119.6(3) . . ?
N9 C53 C54 114.6(3) . . ?
C52 C53 C54 125.8(3) . . ?
N10 C54 C53 112.2(3) . . ?
N10 C54 C55 124.2(3) . . ?
C53 C54 C55 123.5(3) . . ?
C60 C55 C56 118.1(3) . . ?
C60 C55 C54 120.8(3) . . ?
C56 C55 C54 121.1(3) . . ?
C57 C56 C55 120.0(3) . . ?
C57 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?
C58 C57 C56 121.4(4) . . ?
C58 C57 H57 119.3 . . ?
C56 C57 H57 119.3 . . ?
C57 C58 C59 119.8(4) . . ?
C57 C58 H58 120.1 . . ?
C59 C58 H58 120.1 . . ?
C58 C59 C60 120.4(4) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C59 C60 C55 120.3(4) . . ?
C59 C60 H60 119.9 . . ?
C55 C60 H60 119.9 . . ?
N11 C61 C62 123.0(4) . . ?
N11 C61 H61 118.5 . . ?
C62 C61 H61 118.5 . . ?
C61 C62 C63 118.9(4) . . ?
C61 C62 H62 120.6 . . ?
C63 C62 H62 120.6 . . ?
C62 C63 C64 119.5(4) . . ?
C62 C63 H63 120.3 . . ?
C64 C63 H63 120.3 . . ?
C63 C64 C65 118.5(4) . . ?
C63 C64 H64 120.8 . . ?
C65 C64 H64 120.8 . . ?
N11 C65 C64 121.3(3) . . ?
N11 C65 C66 115.3(3) . . ?
C64 C65 C66 123.3(3) . . ?
N12 C66 C65 114.5(3) . . ?
N12 C66 C67 124.5(3) . . ?
C65 C66 C67 121.0(3) . . ?
C72 C67 C68 119.6(4) . . ?
C72 C67 C66 120.4(3) . . ?
C68 C67 C66 119.9(3) . . ?
C69 C68 C67 120.2(4) . . ?
C69 C68 H68 119.9 . . ?
C67 C68 H68 119.9 . . ?
C68 C69 C70 119.9(4) . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C71 C70 C69 120.3(4) . . ?
C71 C70 H70 119.8 . . ?
C69 C70 H70 119.8 . . ?
C70 C71 C72 120.4(4) . . ?
C70 C71 H71 119.8 . . ?
C72 C71 H71 119.8 . . ?
C71 C72 C67 119.3(4) . . ?
C71 C72 H72 120.3 . . ?
C67 C72 H72 120.3 . . ?
C74 C73 H73A 109.5 . . ?
C74 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C74 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
N13 C74 C73 178.7(6) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.260
_refine_diff_density_min -0.939
_refine_diff_density_rms 0.088
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 661 148 ' '
2 0.500 0.500 0.500 661 147 ' '
# start Validation Reply Form
_vrf_CHEMW03_shelxl
;
RESPONSE: The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents (4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT043_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents (4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT041_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT042_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_PLAT068_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_FORMU01_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
_vrf_CELLZ01_shelxl
;
RESPONSE:The reported formula, molecular weight, F000, density etc include
the contribution of disordered solvents(4 CH3CN, 6H2O),
which were removed by SQUEEZE.
;
# end Validation Reply Form