# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr La-Sheng Long'
_publ_contact_author_email       lslong@xmu.edu.cn

_publ_section_title              
;
Magnetic and thermal properties of
three ionothermally synthesized metal-carboxylate
frameworks of [M3(ip)4][EMIm]2
(M = Co, Ni, Mn, H2ip = isophthalic acid, EMIm = 1-ethyl-3-methyl imidazolium)

;
_publ_author_name                'La-Sheng Long'

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 809087'
#TrackingRef '- complex 1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H38 Co3 N4 O16'
_chemical_formula_weight         1055.57

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ORTHORHOMBIC
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.414(3)
_cell_length_b                   11.877(2)
_cell_length_c                   24.154(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4421.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2156
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.7551
_exptl_absorpt_correction_T_max  0.8416
_exptl_absorpt_process_details   Tompa_analytical

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57119
_diffrn_reflns_av_R_equivalents  0.1588
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4335
_reflns_number_gt                2418
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       R-AXIS-SPIDER
_computing_cell_refinement       RAPID
_computing_data_reduction        RAPID
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_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^)+(0.0820P)^2^+1.0272P] 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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4335
_refine_ls_number_parameters     306
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1475
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.011

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
Co1 Co 0.5000 0.5000 0.5000 0.0675(12) Uani 1 2 d S . .
Co2 Co 0.44997(5) 0.64049(6) 0.37531(3) 0.0753(12) Uani 1 1 d . . .
O1 O 0.4283(2) 0.5463(3) 0.56845(14) 0.0815(16) Uani 1 1 d . . .
O2 O 0.4691(3) 0.4810(4) 0.65159(16) 0.0922(17) Uani 1 1 d . . .
O3 O 0.3560(3) 0.9015(4) 0.79954(17) 0.0970(17) Uani 1 1 d . . .
O4 O 0.4458(3) 0.7596(4) 0.80559(16) 0.0897(16) Uani 1 1 d . . .
O5 O 0.3944(2) 0.5474(3) 0.44396(15) 0.0790(15) Uani 1 1 d . . .
O6 O 0.3334(3) 0.7013(4) 0.41325(17) 0.0976(17) Uani 1 1 d . . .
O7 O 0.0558(3) 0.8416(3) 0.50050(15) 0.0818(16) Uani 1 1 d . . .
O8 O 0.0288(3) 0.7584(3) 0.58232(16) 0.0912(17) Uani 1 1 d . . .
C1 C 0.3819(4) 0.6455(5) 0.6477(2) 0.0772(19) Uani 1 1 d . . .
C2 C 0.4020(4) 0.6808(5) 0.7000(2) 0.0783(19) Uani 1 1 d . . .
H2A H 0.4433 0.6415 0.7203 0.094 Uiso 1 1 calc R . .
C3 C 0.3622(4) 0.7740(5) 0.7235(2) 0.0755(19) Uani 1 1 d . . .
C4 C 0.2995(4) 0.8301(5) 0.6935(2) 0.087(2) Uani 1 1 d . . .
H4A H 0.2726 0.8931 0.7086 0.105 Uiso 1 1 calc R . .
C5 C 0.2761(5) 0.7936(6) 0.6412(3) 0.101(2) Uani 1 1 d . . .
H5A H 0.2328 0.8310 0.6217 0.122 Uiso 1 1 calc R . .
C6 C 0.3169(4) 0.7020(6) 0.6179(2) 0.092(2) Uani 1 1 d . . .
H6A H 0.3015 0.6777 0.5826 0.110 Uiso 1 1 calc R . .
C7 C 0.4298(4) 0.5501(5) 0.6202(2) 0.0733(18) Uani 1 1 d . . .
C8 C 0.3894(4) 0.8154(5) 0.7795(2) 0.082(2) Uani 1 1 d . . .
C9 C 0.2545(4) 0.5978(5) 0.4796(2) 0.0752(18) Uani 1 1 d . . .
C10 C 0.1956(4) 0.6831(5) 0.4878(2) 0.0736(18) Uani 1 1 d . . .
H10A H 0.2045 0.7523 0.4707 0.088 Uiso 1 1 calc R . .
C11 C 0.1230(4) 0.6680(5) 0.5211(2) 0.0771(19) Uani 1 1 d . . .
C12 C 0.1076(5) 0.5616(6) 0.5424(3) 0.107(2) Uani 1 1 d . . .
H12A H 0.0581 0.5486 0.5635 0.128 Uiso 1 1 calc R . .
C13 C 0.1649(5) 0.4750(6) 0.5326(4) 0.126(3) Uani 1 1 d . . .
H13A H 0.1536 0.4037 0.5467 0.152 Uiso 1 1 calc R . .
C14 C 0.2396(5) 0.4935(5) 0.5018(3) 0.098(2) Uani 1 1 d . . .
H14A H 0.2791 0.4355 0.4962 0.118 Uiso 1 1 calc R . .
C15 C 0.3312(4) 0.6181(5) 0.4445(2) 0.0768(19) Uani 1 1 d . . .
C16 C 0.0626(4) 0.7632(5) 0.5347(2) 0.0731(18) Uani 1 1 d . . .
C17 C 0.6114(5) 0.6916(8) 0.2426(4) 0.127(3) Uani 1 1 d . . .
H17A H 0.5934 0.6478 0.2724 0.153 Uiso 1 1 calc R . .
C18 C 0.6489(12) 0.7447(10) 0.1605(5) 0.245(9) Uani 1 1 d . . .
H18A H 0.6611 0.7427 0.1228 0.294 Uiso 1 1 calc R . .
C19 C 0.6490(8) 0.8353(8) 0.1930(5) 0.166(5) Uani 1 1 d . . .
H19A H 0.6631 0.9084 0.1827 0.199 Uiso 1 1 calc R . .
C20 C 0.6192(6) 0.8701(7) 0.2921(4) 0.144(3) Uani 1 1 d . . .
H20A H 0.6002 0.8254 0.3229 0.216 Uiso 1 1 calc R . .
H20B H 0.5784 0.9298 0.2857 0.216 Uiso 1 1 calc R . .
H20C H 0.6752 0.9017 0.3001 0.216 Uiso 1 1 calc R . .
C21 C 0.6432(10) 0.5288(12) 0.1760(5) 0.224(6) Uani 1 1 d DU . .
H21A H 0.7011 0.5166 0.1615 0.268 Uiso 1 1 calc R . .
H21B H 0.6322 0.4770 0.2063 0.268 Uiso 1 1 calc R . .
C22 C 0.5793(9) 0.5223(11) 0.1346(5) 0.206(6) Uani 1 1 d DU . .
H22A H 0.5790 0.4479 0.1190 0.308 Uiso 1 1 calc R . .
H22B H 0.5918 0.5762 0.1061 0.308 Uiso 1 1 calc R . .
H22C H 0.5235 0.5382 0.1505 0.308 Uiso 1 1 calc R . .
N1 N 0.6250(4) 0.8005(6) 0.2436(3) 0.116(2) Uani 1 1 d . . .
N2 N 0.6274(7) 0.6558(6) 0.1932(4) 0.169(4) Uani 1 1 d . . .

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
Co1 0.0715(14) 0.0732(13) 0.0579(13) -0.0009(4) 0.0005(4) -0.0010(5)
Co2 0.0826(13) 0.0833(13) 0.0599(13) 0.0021(3) -0.0015(4) 0.0016(4)
O1 0.076(3) 0.104(3) 0.064(2) -0.0052(19) 0.0014(17) 0.010(2)
O2 0.106(3) 0.105(3) 0.066(3) -0.002(2) 0.001(2) 0.022(2)
O3 0.121(4) 0.088(3) 0.082(3) -0.014(2) -0.001(2) 0.002(3)
O4 0.095(3) 0.104(3) 0.070(3) -0.009(2) -0.009(2) 0.004(2)
O5 0.076(3) 0.082(3) 0.078(3) -0.0023(18) -0.0009(18) 0.005(2)
O6 0.096(3) 0.112(3) 0.084(3) 0.026(3) 0.009(2) 0.019(2)
O7 0.096(3) 0.082(3) 0.068(3) 0.0009(19) 0.0112(19) 0.009(2)
O8 0.106(3) 0.094(3) 0.074(3) 0.010(2) 0.013(2) 0.012(2)
C1 0.076(4) 0.089(4) 0.066(3) -0.004(3) 0.004(3) 0.008(3)
C2 0.087(4) 0.086(4) 0.062(3) 0.000(3) -0.003(3) 0.002(3)
C3 0.081(4) 0.086(4) 0.060(3) -0.008(3) 0.002(3) -0.004(3)
C4 0.096(4) 0.088(4) 0.078(4) -0.005(3) 0.000(3) 0.008(3)
C5 0.113(5) 0.111(5) 0.080(4) -0.011(4) -0.018(4) 0.028(4)
C6 0.098(5) 0.107(5) 0.071(4) -0.010(3) -0.011(3) 0.021(4)
C7 0.078(4) 0.081(4) 0.061(3) -0.003(3) 0.001(3) -0.002(3)
C8 0.089(4) 0.084(4) 0.072(4) -0.005(3) 0.000(3) -0.008(3)
C9 0.078(4) 0.079(4) 0.069(3) 0.002(3) 0.001(3) 0.007(3)
C10 0.075(4) 0.077(3) 0.068(3) 0.005(3) -0.006(3) 0.000(3)
C11 0.076(4) 0.080(4) 0.075(3) 0.005(3) 0.007(3) 0.008(3)
C12 0.090(5) 0.094(5) 0.136(6) 0.019(4) 0.034(4) 0.013(4)
C13 0.118(6) 0.094(5) 0.167(8) 0.037(5) 0.035(6) 0.016(4)
C14 0.098(5) 0.076(4) 0.121(5) 0.006(4) 0.011(4) 0.017(3)
C15 0.076(4) 0.093(4) 0.061(3) -0.004(3) -0.007(3) 0.009(3)
C16 0.073(4) 0.084(4) 0.062(3) 0.005(3) 0.004(3) -0.001(3)
C17 0.117(6) 0.110(7) 0.155(8) -0.004(6) 0.026(5) 0.005(5)
C18 0.42(2) 0.122(8) 0.191(11) -0.009(8) 0.187(14) -0.009(11)
C19 0.202(11) 0.102(6) 0.195(10) -0.005(7) 0.100(9) -0.004(6)
C20 0.151(8) 0.121(6) 0.160(9) -0.016(6) -0.019(6) -0.012(6)
C21 0.234(15) 0.199(13) 0.238(15) 0.077(11) -0.019(13) -0.040(11)
C22 0.211(11) 0.201(11) 0.205(11) 0.026(8) -0.056(9) -0.083(9)
N1 0.091(4) 0.096(5) 0.161(7) -0.001(4) 0.019(4) 0.006(3)
N2 0.244(10) 0.090(5) 0.174(8) -0.002(5) 0.093(7) -0.012(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
Co1 O1 2.064(3) . ?
Co1 O1 2.064(3) 5_666 ?
Co1 O7 2.069(4) 4_566 ?
Co1 O7 2.069(4) 8_655 ?
Co1 O5 2.191(4) 5_666 ?
Co1 O5 2.191(4) . ?
Co2 O8 1.991(4) 4_566 ?
Co2 O2 2.016(4) 5_666 ?
Co2 O4 2.061(4) 7_575 ?
Co2 O6 2.143(4) . ?
Co2 O5 2.169(4) . ?
Co2 O3 2.386(4) 7_575 ?
Co2 C15 2.493(6) . ?
O1 C7 1.251(6) . ?
O2 C7 1.271(7) . ?
O2 Co2 2.016(4) 5_666 ?
O3 C8 1.242(7) . ?
O3 Co2 2.386(4) 7_576 ?
O4 C8 1.262(7) . ?
O4 Co2 2.061(4) 7_576 ?
O5 C15 1.286(6) . ?
O6 C15 1.244(7) . ?
O7 C16 1.248(6) . ?
O7 Co1 2.069(4) 4_466 ?
O8 C16 1.265(6) . ?
O8 Co2 1.991(4) 4_466 ?
C1 C2 1.367(7) . ?
C1 C6 1.405(8) . ?
C1 C7 1.507(8) . ?
C2 C3 1.386(8) . ?
C3 C4 1.380(8) . ?
C3 C8 1.500(8) . ?
C4 C5 1.383(8) . ?
C5 C6 1.375(8) . ?
C9 C14 1.369(8) . ?
C9 C10 1.375(7) . ?
C9 C15 1.474(8) . ?
C10 C11 1.390(8) . ?
C11 C12 1.385(8) . ?
C11 C16 1.500(8) . ?
C12 C13 1.377(9) . ?
C13 C14 1.388(10) . ?
C17 N2 1.290(10) . ?
C17 N1 1.310(9) . ?
C18 C19 1.331(13) . ?
C18 N2 1.360(12) . ?
C19 N1 1.341(10) . ?
C20 N1 1.437(10) . ?
C21 C22 1.406(9) . ?
C21 N2 1.584(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
O1 Co1 O1 180.00(12) . 5_666 ?
O1 Co1 O7 89.12(16) . 4_566 ?
O1 Co1 O7 90.88(16) 5_666 4_566 ?
O1 Co1 O7 90.88(16) . 8_655 ?
O1 Co1 O7 89.12(16) 5_666 8_655 ?
O7 Co1 O7 180.0 4_566 8_655 ?
O1 Co1 O5 88.37(14) . 5_666 ?
O1 Co1 O5 91.63(14) 5_666 5_666 ?
O7 Co1 O5 85.92(14) 4_566 5_666 ?
O7 Co1 O5 94.08(14) 8_655 5_666 ?
O1 Co1 O5 91.63(14) . . ?
O1 Co1 O5 88.37(14) 5_666 . ?
O7 Co1 O5 94.08(14) 4_566 . ?
O7 Co1 O5 85.92(14) 8_655 . ?
O5 Co1 O5 180.000(1) 5_666 . ?
O8 Co2 O2 102.67(19) 4_566 5_666 ?
O8 Co2 O4 95.27(16) 4_566 7_575 ?
O2 Co2 O4 99.68(17) 5_666 7_575 ?
O8 Co2 O6 95.12(18) 4_566 . ?
O2 Co2 O6 153.95(19) 5_666 . ?
O4 Co2 O6 97.43(16) 7_575 . ?
O8 Co2 O5 98.93(15) 4_566 . ?
O2 Co2 O5 97.25(16) 5_666 . ?
O4 Co2 O5 154.91(17) 7_575 . ?
O6 Co2 O5 60.88(15) . . ?
O8 Co2 O3 152.93(16) 4_566 7_575 ?
O2 Co2 O3 88.78(16) 5_666 7_575 ?
O4 Co2 O3 58.32(16) 7_575 7_575 ?
O6 Co2 O3 83.65(16) . 7_575 ?
O5 Co2 O3 103.90(15) . 7_575 ?
O8 Co2 C15 99.69(17) 4_566 . ?
O2 Co2 C15 126.5(2) 5_666 . ?
O4 Co2 C15 125.88(18) 7_575 . ?
O6 Co2 C15 29.92(16) . . ?
O5 Co2 C15 31.04(16) . . ?
O3 Co2 C15 92.63(17) 7_575 . ?
C7 O1 Co1 143.1(4) . . ?
C7 O2 Co2 124.4(4) . 5_666 ?
C8 O3 Co2 82.9(4) . 7_576 ?
C8 O4 Co2 97.3(4) . 7_576 ?
C15 O5 Co2 88.5(3) . . ?
C15 O5 Co1 136.5(3) . . ?
Co2 O5 Co1 108.06(16) . . ?
C15 O6 Co2 90.8(4) . . ?
C16 O7 Co1 135.8(3) . 4_466 ?
C16 O8 Co2 133.8(4) . 4_466 ?
C2 C1 C6 119.3(5) . . ?
C2 C1 C7 121.8(5) . . ?
C6 C1 C7 118.9(5) . . ?
C1 C2 C3 121.5(5) . . ?
C4 C3 C2 118.8(5) . . ?
C4 C3 C8 120.7(5) . . ?
C2 C3 C8 120.5(5) . . ?
C3 C4 C5 120.7(6) . . ?
C6 C5 C4 120.2(6) . . ?
C5 C6 C1 119.6(6) . . ?
O1 C7 O2 125.6(5) . . ?
O1 C7 C1 117.3(5) . . ?
O2 C7 C1 117.1(5) . . ?
O3 C8 O4 121.5(5) . . ?
O3 C8 C3 120.4(6) . . ?
O4 C8 C3 118.1(5) . . ?
C14 C9 C10 119.9(6) . . ?
C14 C9 C15 120.5(5) . . ?
C10 C9 C15 119.5(5) . . ?
C9 C10 C11 121.4(5) . . ?
C12 C11 C10 118.1(5) . . ?
C12 C11 C16 120.0(5) . . ?
C10 C11 C16 121.9(5) . . ?
C13 C12 C11 120.5(6) . . ?
C12 C13 C14 120.5(7) . . ?
C9 C14 C13 119.5(6) . . ?
O6 C15 O5 119.5(5) . . ?
O6 C15 C9 120.0(5) . . ?
O5 C15 C9 120.5(5) . . ?
O6 C15 Co2 59.2(3) . . ?
O5 C15 Co2 60.4(3) . . ?
C9 C15 Co2 172.6(4) . . ?
O7 C16 O8 126.9(5) . . ?
O7 C16 C11 118.1(5) . . ?
O8 C16 C11 114.8(5) . . ?
N2 C17 N1 108.2(8) . . ?
C19 C18 N2 106.6(9) . . ?
C18 C19 N1 106.7(9) . . ?
C22 C21 N2 97.5(11) . . ?
C17 N1 C19 109.4(8) . . ?
C17 N1 C20 124.9(9) . . ?
C19 N1 C20 125.6(8) . . ?
C17 N2 C18 109.1(8) . . ?
C17 N2 C21 125.9(9) . . ?
C18 N2 C21 123.4(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.043

# Attachment '- complex 2-Revised.cif'

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 809088'
#TrackingRef '- complex 2-Revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H38 N4 Ni3 O16'
_chemical_formula_weight         1054.91

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ORTHORHOMBIC
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.4912(6)
_cell_length_b                   11.6687(5)
_cell_length_c                   23.7502(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4293.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2168
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7695
_exptl_absorpt_correction_T_max  0.8195
_exptl_absorpt_process_details   'CrysAlis RED'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Oxford Gemini S Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12466
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4206
_reflns_number_gt                2569
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_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^)+(0.0241P)^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_number_reflns         4206
_refine_ls_number_parameters     350
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.004
_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 0.0000 0.5000 0.0000 0.01116(10) Uani 1 2 d S . .
Ni2 Ni 0.046976(19) 0.35733(3) 0.123107(12) 0.01617(8) Uani 1 1 d . . .
O1 O 0.15795(11) 0.28741(14) 0.08386(7) 0.0236(5) Uani 1 1 d . . .
O2 O 0.09892(10) 0.44945(13) 0.05684(6) 0.0148(4) Uani 1 1 d . . .
O3 O 0.44279(9) 0.15831(13) 0.00153(6) 0.0188(4) Uani 1 1 d . . .
O4 O 0.46705(11) 0.24271(14) -0.08198(6) 0.0248(5) Uani 1 1 d . . .
O5 O 0.13573(11) 0.40019(15) 0.19449(7) 0.0267(5) Uani 1 1 d . . .
O6 O 0.04714(11) 0.25446(14) 0.19290(6) 0.0238(5) Uani 1 1 d . . .
O7 O 0.07311(10) 0.05096(14) 0.43320(6) 0.0179(5) Uani 1 1 d . . .
O8 O 0.03919(11) -0.02815(14) 0.34941(6) 0.0245(5) Uani 1 1 d . . .
C1 C 0.23919(15) 0.3999(2) 0.01992(9) 0.0152(6) Uani 1 1 d . . .
C2 C 0.30005(15) 0.3142(2) 0.01263(9) 0.0149(7) Uani 1 1 d . . .
H2A H 0.2918 0.2435 0.0299 0.018 Uiso 1 1 calc R . .
C3 C 0.37295(15) 0.3320(2) -0.01998(10) 0.0153(7) Uani 1 1 d . . .
C4 C 0.38650(17) 0.4414(2) -0.04224(12) 0.0302(8) Uani 1 1 d . . .
H4A H 0.4355 0.4558 -0.0637 0.036 Uiso 1 1 calc R . .
C5 C 0.32794(17) 0.5281(2) -0.03268(13) 0.0383(9) Uani 1 1 d . . .
H5A H 0.3391 0.6013 -0.0462 0.046 Uiso 1 1 calc R . .
C6 C 0.25214(15) 0.5069(2) -0.00286(11) 0.0269(7) Uani 1 1 d . . .
H6A H 0.2110 0.5642 0.0016 0.032 Uiso 1 1 calc R . .
C7 C 0.16141(15) 0.3762(2) 0.05426(10) 0.0136(6) Uani 1 1 d . . .
C8 C 0.43357(15) 0.2351(2) -0.03399(10) 0.0147(7) Uani 1 1 d . . .
C9 C 0.13657(16) 0.2727(2) 0.27316(10) 0.0199(7) Uani 1 1 d . . .
C10 C 0.09919(16) 0.1768(2) 0.29827(10) 0.0196(7) Uani 1 1 d . . .
H10A H 0.0575 0.1354 0.2788 0.024 Uiso 1 1 calc R . .
C11 C 0.12315(15) 0.1423(2) 0.35179(9) 0.0185(7) Uani 1 1 d . . .
C12 C 0.18702(16) 0.2018(2) 0.37903(11) 0.0262(7) Uani 1 1 d . . .
H12A H 0.2037 0.1790 0.4149 0.031 Uiso 1 1 calc R . .
C13 C 0.22717(17) 0.2951(2) 0.35431(11) 0.0299(8) Uani 1 1 d . . .
H13A H 0.2711 0.3335 0.3731 0.036 Uiso 1 1 calc R . .
C14 C 0.20131(17) 0.3306(2) 0.30123(10) 0.0245(8) Uani 1 1 d . . .
H14A H 0.2276 0.3936 0.2845 0.029 Uiso 1 1 calc R . .
C15 C 0.10644(15) 0.3121(2) 0.21641(9) 0.0101(6) Uani 1 1 d U . .
C16 C 0.07498(15) 0.0463(2) 0.38063(11) 0.0178(7) Uani 1 1 d . . .
C17 C -0.10551(19) 0.3138(2) 0.26368(14) 0.0573(11) Uani 1 1 d D . .
H17A H -0.0923 0.3586 0.2309 0.069 Uiso 1 1 d R A .
N1 N -0.12198(16) 0.2017(2) 0.26300(12) 0.0590(9) Uani 1 1 d D A .
C20 C -0.1248(2) 0.1292(3) 0.21362(15) 0.0728(13) Uani 1 1 d . . .
H20A H -0.1146 0.1747 0.1806 0.109 Uiso 1 1 calc R A .
H20B H -0.1806 0.0937 0.2110 0.109 Uiso 1 1 calc R . .
H20C H -0.0812 0.0711 0.2165 0.109 Uiso 1 1 calc R . .
C19 C -0.1141(3) 0.1667(4) 0.3253(2) 0.0239(15) Uani 0.50 1 d PDU A 1
H19A H -0.1204 0.0922 0.3386 0.029 Uiso 0.50 1 calc PR A 1
N2 N -0.0862(3) 0.3501(4) 0.32464(18) 0.0280(13) Uani 0.50 1 d PDU A 1
C18 C -0.0971(3) 0.2563(4) 0.3573(2) 0.0221(14) Uani 0.50 1 d PDU A 1
H18A H -0.0933 0.2551 0.3964 0.027 Uiso 0.50 1 calc PR A 1
C21 C -0.0690(4) 0.4660(5) 0.3449(3) 0.047(2) Uani 0.50 1 d PDU A 1
H21A H -0.0347 0.5084 0.3178 0.056 Uiso 0.50 1 calc PR A 1
H21B H -0.0385 0.4641 0.3805 0.056 Uiso 0.50 1 calc PR A 1
C22 C -0.1624(5) 0.5234(7) 0.3523(4) 0.112(3) Uani 0.50 1 d PDU A 1
H22A H -0.1578 0.5896 0.3761 0.168 Uiso 0.50 1 calc PR A 1
H22B H -0.2011 0.4691 0.3691 0.168 Uiso 0.50 1 calc PR A 1
H22C H -0.1842 0.5460 0.3161 0.168 Uiso 0.50 1 calc PR A 1
C18' C -0.1724(5) 0.2557(6) 0.3368(3) 0.082(3) Uani 0.50 1 d PDU A 2
H18B H -0.1941 0.2583 0.3733 0.098 Uiso 0.50 1 calc PR A 2
C19' C -0.1646(5) 0.1622(6) 0.3033(3) 0.073(3) Uani 0.50 1 d PDU A 2
H19B H -0.1853 0.0882 0.3088 0.088 Uiso 0.50 1 calc PR A 2
N2' N -0.1404(4) 0.3485(4) 0.3047(2) 0.0560(18) Uani 0.50 1 d PDU A 2
C21' C -0.1331(6) 0.4657(6) 0.3234(3) 0.087(3) Uani 0.50 1 d PDU A 2
H21C H -0.1021 0.5067 0.2942 0.104 Uiso 0.50 1 calc PR A 2
H21D H -0.1912 0.4968 0.3239 0.104 Uiso 0.50 1 calc PR A 2
C22' C -0.0940(4) 0.4966(6) 0.3756(3) 0.059(2) Uani 0.50 1 d PDU A 2
H22D H -0.1181 0.5677 0.3886 0.089 Uiso 0.50 1 calc PR A 2
H22E H -0.0329 0.5053 0.3704 0.089 Uiso 0.50 1 calc PR A 2
H22F H -0.1048 0.4377 0.4029 0.089 Uiso 0.50 1 calc PR A 2

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 0.01375(19) 0.0116(2) 0.00809(19) -0.0001(2) -0.0002(2) 0.0010(2)
Ni2 0.02006(15) 0.01826(16) 0.01019(14) 0.00193(16) -0.00116(17) 0.00391(18)
O1 0.0295(10) 0.0203(10) 0.0210(10) 0.0061(9) 0.0062(9) 0.0102(9)
O2 0.0162(9) 0.0169(9) 0.0115(9) -0.0004(8) -0.0023(8) 0.0029(8)
O3 0.0228(9) 0.0161(9) 0.0176(8) 0.0008(8) 0.0044(9) 0.0044(8)
O4 0.0303(10) 0.0252(10) 0.0190(9) 0.0089(8) 0.0078(9) 0.0062(9)
O5 0.0396(11) 0.0233(10) 0.0173(9) 0.0040(9) -0.0043(10) 0.0006(9)
O6 0.0238(9) 0.0343(11) 0.0133(9) 0.0076(8) -0.0017(9) 0.0014(10)
O7 0.0188(9) 0.0253(10) 0.0097(9) 0.0033(8) -0.0019(8) -0.0045(8)
O8 0.0332(10) 0.0289(11) 0.0112(8) -0.0001(8) 0.0006(9) -0.0141(9)
C1 0.0163(13) 0.0166(14) 0.0128(12) 0.0006(11) -0.0023(12) 0.0046(12)
C2 0.0233(13) 0.0100(13) 0.0113(13) 0.0013(11) -0.0020(12) 0.0038(12)
C3 0.0154(12) 0.0173(15) 0.0133(13) 0.0016(11) 0.0017(12) 0.0025(12)
C4 0.0230(14) 0.0247(16) 0.0430(18) 0.0099(15) 0.0174(15) 0.0048(14)
C5 0.0402(17) 0.0120(16) 0.063(2) 0.0176(15) 0.0196(18) 0.0023(14)
C6 0.0271(13) 0.0153(13) 0.0383(15) 0.0059(14) 0.0040(16) 0.0086(15)
C7 0.0144(12) 0.0143(14) 0.0120(13) -0.0030(12) -0.0054(11) 0.0002(12)
C8 0.0114(13) 0.0162(14) 0.0164(13) -0.0023(12) -0.0016(12) -0.0035(12)
C9 0.0222(14) 0.0222(16) 0.0154(14) 0.0038(12) 0.0009(13) 0.0030(13)
C10 0.0197(13) 0.0252(16) 0.0139(13) 0.0007(12) 0.0008(13) -0.0030(13)
C11 0.0238(13) 0.0235(15) 0.0082(12) 0.0047(13) -0.0020(12) -0.0027(14)
C12 0.0295(14) 0.0325(16) 0.0167(13) 0.0114(14) -0.0048(15) -0.0091(14)
C13 0.0313(16) 0.0349(17) 0.0235(15) 0.0023(14) -0.0077(14) -0.0187(15)
C14 0.0314(15) 0.0193(16) 0.0229(14) 0.0064(13) 0.0009(15) -0.0069(14)
C15 0.0143(12) 0.0119(13) 0.0042(11) 0.0047(10) -0.0011(11) 0.0056(11)
C16 0.0142(12) 0.0215(14) 0.0176(13) 0.0069(13) -0.0048(13) -0.0012(12)
C17 0.051(2) 0.034(2) 0.087(3) 0.0082(19) 0.043(2) 0.0078(18)
N1 0.0446(16) 0.0267(15) 0.106(2) -0.0040(17) 0.0336(18) 0.0047(14)
C20 0.059(2) 0.044(2) 0.115(3) 0.005(2) -0.037(2) -0.009(2)
C19 0.017(2) 0.023(3) 0.032(3) 0.006(2) 0.014(3) 0.001(2)
N2 0.018(2) 0.028(3) 0.038(3) -0.009(2) 0.004(2) 0.002(2)
C18 0.021(3) 0.023(3) 0.023(3) 0.001(2) 0.012(2) 0.002(3)
C21 0.066(4) 0.025(3) 0.050(4) -0.012(3) -0.018(4) -0.026(3)
C22 0.143(6) 0.075(5) 0.117(6) -0.013(5) 0.046(5) -0.023(5)
C18' 0.121(6) 0.050(4) 0.074(5) 0.006(4) 0.043(5) -0.001(4)
C19' 0.083(5) 0.063(5) 0.073(5) 0.002(4) 0.037(4) -0.013(4)
N2' 0.077(4) 0.032(3) 0.059(3) -0.002(3) 0.030(3) -0.006(3)
C21' 0.123(6) 0.062(5) 0.075(5) -0.012(4) 0.047(5) 0.001(5)
C22' 0.061(4) 0.061(4) 0.055(4) 0.010(4) -0.035(4) -0.026(4)

_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 O7 2.0380(15) 7_565 ?
Ni1 O7 2.0380(15) 3 ?
Ni1 O3 2.0492(15) 4_455 ?
Ni1 O3 2.0492(15) 8_665 ?
Ni1 O2 2.1258(15) . ?
Ni1 O2 2.1258(15) 5_565 ?
Ni2 O4 1.9622(17) 4_455 ?
Ni2 O8 1.9983(17) 3 ?
Ni2 O6 2.0466(16) . ?
Ni2 O2 2.0687(15) . ?
Ni2 O1 2.1189(17) . ?
Ni2 O5 2.2393(17) . ?
Ni2 C7 2.422(2) . ?
Ni2 C15 2.457(2) . ?
O1 C7 1.253(3) . ?
O2 C7 1.293(3) . ?
O3 C8 1.239(3) . ?
O3 Ni1 2.0492(15) 4 ?
O4 C8 1.255(3) . ?
O4 Ni2 1.9622(17) 4 ?
O5 C15 1.238(3) . ?
O6 C15 1.268(3) . ?
O7 C16 1.250(3) . ?
O7 Ni1 2.0380(15) 3_545 ?
O8 C16 1.270(3) . ?
O8 Ni2 1.9983(17) 3_545 ?
C1 C6 1.376(3) . ?
C1 C2 1.386(3) . ?
C1 C7 1.481(3) . ?
C2 C3 1.385(3) . ?
C3 C4 1.397(3) . ?
C3 C8 1.507(3) . ?
C4 C5 1.378(4) . ?
C5 C6 1.393(3) . ?
C9 C14 1.381(3) . ?
C9 C10 1.394(3) . ?
C9 C15 1.499(3) . ?
C10 C11 1.384(3) . ?
C11 C12 1.371(3) . ?
C11 C16 1.510(3) . ?
C12 C13 1.384(3) . ?
C13 C14 1.386(3) . ?
C17 N2' 1.185(6) . ?
C17 N1 1.333(4) . ?
C17 N2 1.538(5) . ?
N1 C19' 1.251(7) . ?
N1 C20 1.446(4) . ?
N1 C19 1.540(5) . ?
C19 C18 1.319(6) . ?
N2 C18 1.353(6) . ?
N2 C21 1.460(6) . ?
C21 C22 1.603(9) . ?
C18' C19' 1.357(8) . ?
C18' N2' 1.414(8) . ?
N2' C21' 1.442(8) . ?
C21' C22' 1.427(9) . ?

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 Ni1 O7 180.00(9) 7_565 3 ?
O7 Ni1 O3 87.91(6) 7_565 4_455 ?
O7 Ni1 O3 92.09(6) 3 4_455 ?
O7 Ni1 O3 92.09(6) 7_565 8_665 ?
O7 Ni1 O3 87.91(6) 3 8_665 ?
O3 Ni1 O3 180.00(4) 4_455 8_665 ?
O7 Ni1 O2 90.74(6) 7_565 . ?
O7 Ni1 O2 89.26(6) 3 . ?
O3 Ni1 O2 94.18(6) 4_455 . ?
O3 Ni1 O2 85.82(6) 8_665 . ?
O7 Ni1 O2 89.26(6) 7_565 5_565 ?
O7 Ni1 O2 90.74(6) 3 5_565 ?
O3 Ni1 O2 85.82(6) 4_455 5_565 ?
O3 Ni1 O2 94.18(6) 8_665 5_565 ?
O2 Ni1 O2 180.00(6) . 5_565 ?
O4 Ni2 O8 97.99(7) 4_455 3 ?
O4 Ni2 O6 93.15(7) 4_455 . ?
O8 Ni2 O6 97.38(7) 3 . ?
O4 Ni2 O2 100.13(6) 4_455 . ?
O8 Ni2 O2 99.26(6) 3 . ?
O6 Ni2 O2 156.99(7) . . ?
O4 Ni2 O1 93.66(7) 4_455 . ?
O8 Ni2 O1 160.58(7) 3 . ?
O6 Ni2 O1 97.44(7) . . ?
O2 Ni2 O1 63.25(6) . . ?
O4 Ni2 O5 153.79(7) 4_455 . ?
O8 Ni2 O5 90.78(7) 3 . ?
O6 Ni2 O5 61.12(6) . . ?
O2 Ni2 O5 102.77(6) . . ?
O1 Ni2 O5 85.46(6) . . ?
O4 Ni2 C7 100.36(7) 4_455 . ?
O8 Ni2 C7 130.45(8) 3 . ?
O6 Ni2 C7 126.82(8) . . ?
O2 Ni2 C7 32.26(7) . . ?
O1 Ni2 C7 31.14(7) . . ?
O5 Ni2 C7 92.37(7) . . ?
O4 Ni2 C15 123.90(7) 4_455 . ?
O8 Ni2 C15 95.71(7) 3 . ?
O6 Ni2 C15 31.04(7) . . ?
O2 Ni2 C15 130.68(7) . . ?
O1 Ni2 C15 90.56(7) . . ?
O5 Ni2 C15 30.12(7) . . ?
C7 Ni2 C15 110.73(8) . . ?
C7 O1 Ni2 87.89(14) . . ?
C7 O2 Ni2 89.07(13) . . ?
C7 O2 Ni1 133.87(14) . . ?
Ni2 O2 Ni1 110.30(7) . . ?
C8 O3 Ni1 133.63(15) . 4 ?
C8 O4 Ni2 132.12(16) . 4 ?
C15 O5 Ni2 84.72(14) . . ?
C15 O6 Ni2 92.65(14) . . ?
C16 O7 Ni1 141.06(16) . 3_545 ?
C16 O8 Ni2 123.96(15) . 3_545 ?
C6 C1 C2 120.5(2) . . ?
C6 C1 C7 120.3(2) . . ?
C2 C1 C7 119.2(2) . . ?
C3 C2 C1 121.0(2) . . ?
C2 C3 C4 118.2(2) . . ?
C2 C3 C8 121.2(2) . . ?
C4 C3 C8 120.5(2) . . ?
C5 C4 C3 120.6(2) . . ?
C4 C5 C6 120.6(2) . . ?
C1 C6 C5 118.9(2) . . ?
O1 C7 O2 119.2(2) . . ?
O1 C7 C1 119.9(2) . . ?
O2 C7 C1 120.8(2) . . ?
O1 C7 Ni2 60.97(12) . . ?
O2 C7 Ni2 58.66(11) . . ?
C1 C7 Ni2 169.84(17) . . ?
O3 C8 O4 128.4(2) . . ?
O3 C8 C3 117.7(2) . . ?
O4 C8 C3 113.9(2) . . ?
C14 C9 C10 119.2(2) . . ?
C14 C9 C15 120.7(2) . . ?
C10 C9 C15 120.1(2) . . ?
C11 C10 C9 121.0(2) . . ?
C12 C11 C10 118.7(2) . . ?
C12 C11 C16 121.2(2) . . ?
C10 C11 C16 120.0(2) . . ?
C11 C12 C13 121.5(2) . . ?
C12 C13 C14 119.4(2) . . ?
C9 C14 C13 120.2(2) . . ?
O5 C15 O6 121.4(2) . . ?
O5 C15 C9 121.3(2) . . ?
O6 C15 C9 117.3(2) . . ?
O5 C15 Ni2 65.16(12) . . ?
O6 C15 Ni2 56.31(11) . . ?
C9 C15 Ni2 173.57(18) . . ?
O7 C16 O8 127.0(2) . . ?
O7 C16 C11 115.6(2) . . ?
O8 C16 C11 117.3(2) . . ?
N2' C17 N1 105.0(4) . . ?
N2' C17 N2 38.8(3) . . ?
N1 C17 N2 108.6(3) . . ?
C19' N1 C17 117.0(4) . . ?
C19' N1 C20 112.9(4) . . ?
C17 N1 C20 126.1(3) . . ?
C19' N1 C19 37.7(4) . . ?
C17 N1 C19 103.5(3) . . ?
C20 N1 C19 128.8(3) . . ?
C18 C19 N1 111.1(4) . . ?
C18 N2 C21 125.8(5) . . ?
C18 N2 C17 107.0(3) . . ?
C21 N2 C17 126.9(4) . . ?
C19 C18 N2 109.6(4) . . ?
N2 C21 C22 105.0(5) . . ?
C19' C18' N2' 105.6(5) . . ?
N1 C19' C18' 101.5(5) . . ?
C17 N2' C18' 110.0(5) . . ?
C17 N2' C21' 122.8(5) . . ?
C18' N2' C21' 126.0(6) . . ?
C22' C21' N2' 122.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.080

# complex2 RESULTS (APPEND TO CIF)

_vrf_PLAT223_complex2            
;
PROBLEM: Large Solvent/Anion H Ueq(max)/Ueq(min) ... 6.22 Ratio

RESPONSE: This is caused by disordered
C18 C19 N2 C21 C22 of 1-ethyl-3-methyl-imidazolium.
;

# end Validation Reply Form


# Attachment '- complex 3.cif'

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 809089'
#TrackingRef '- complex 3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H38 Mn3 N4 O16'
_chemical_formula_weight         1043.60

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'

_symmetry_cell_setting           MONOCLINIC
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.092(3)
_cell_length_b                   14.490(3)
_cell_length_c                   12.640(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.85(3)
_cell_angle_gamma                90.00
_cell_volume                     2139.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1066
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.8473
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_process_details   Tompa_analytical

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17947
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4195
_reflns_number_gt                2903
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       R-AXIS-SPIDER
_computing_cell_refinement       RAPID
_computing_data_reduction        RAPID
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_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^)+(0.0741P)^2^+2.4336P] 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_number_reflns         4195
_refine_ls_number_parameters     304
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1795
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.153
_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
Mn1 Mn 0.0000 0.5000 0.0000 0.0183(3) Uani 1 2 d S . .
Mn2 Mn 0.27135(5) 0.44289(4) 0.24477(6) 0.0200(2) Uani 1 1 d . . .
O1 O 0.0285(3) 0.5569(2) 0.1717(3) 0.0303(8) Uani 1 1 d . . .
O2 O 0.1816(3) 0.5010(2) 0.3283(3) 0.0296(8) Uani 1 1 d . . .
O3 O -0.1928(3) 0.8047(2) 0.2452(3) 0.0257(7) Uani 1 1 d . . .
O4 O -0.1164(2) 0.8817(2) 0.4131(3) 0.0221(7) Uani 1 1 d . . .
O5 O 0.1442(3) 0.5735(2) 0.0055(3) 0.0304(8) Uani 1 1 d . . .
O6 O 0.3079(3) 0.5609(2) 0.1722(3) 0.0272(8) Uani 1 1 d . . .
O7 O 0.5839(3) 0.8351(2) 0.2554(3) 0.0261(8) Uani 1 1 d . . .
O8 O 0.5740(3) 0.9109(2) 0.0993(3) 0.0267(8) Uani 1 1 d . . .
C1 C 0.0642(4) 0.6059(3) 0.3650(4) 0.0249(10) Uani 1 1 d . . .
C2 C -0.0140(4) 0.6776(3) 0.3221(4) 0.0206(10) Uani 1 1 d . . .
H2A H -0.0554 0.6865 0.2408 0.025 Uiso 1 1 calc R . .
C3 C -0.0314(4) 0.7367(3) 0.4002(4) 0.0245(10) Uani 1 1 d . . .
C4 C 0.0282(4) 0.7230(3) 0.5220(5) 0.0293(11) Uani 1 1 d . . .
H4A H 0.0174 0.7624 0.5743 0.035 Uiso 1 1 calc R . .
C5 C 0.1048(5) 0.6486(4) 0.5644(5) 0.0386(13) Uani 1 1 d . . .
H5A H 0.1444 0.6376 0.6455 0.046 Uiso 1 1 calc R . .
C6 C 0.1217(5) 0.5917(4) 0.4864(5) 0.0352(13) Uani 1 1 d . . .
H6A H 0.1728 0.5426 0.5159 0.042 Uiso 1 1 calc R . .
C7 C 0.0912(4) 0.5490(3) 0.2808(4) 0.0235(10) Uani 1 1 d . . .
C8 C -0.1180(4) 0.8126(3) 0.3496(4) 0.0238(10) Uani 1 1 d . . .
C9 C 0.2934(4) 0.6747(3) 0.0303(4) 0.0212(10) Uani 1 1 d . . .
C10 C 0.3919(4) 0.7229(3) 0.1076(4) 0.0202(9) Uani 1 1 d . . .
H10A H 0.4290 0.7070 0.1875 0.024 Uiso 1 1 calc R . .
C11 C 0.4345(4) 0.7945(3) 0.0653(4) 0.0227(10) Uani 1 1 d . . .
C12 C 0.3799(4) 0.8161(3) -0.0560(4) 0.0259(11) Uani 1 1 d . . .
H12A H 0.4089 0.8629 -0.0850 0.031 Uiso 1 1 calc R . .
C13 C 0.2834(4) 0.7682(3) -0.1325(5) 0.0314(12) Uani 1 1 d . . .
H13A H 0.2480 0.7821 -0.2130 0.038 Uiso 1 1 calc R . .
C14 C 0.2395(4) 0.6989(3) -0.0884(4) 0.0261(11) Uani 1 1 d . . .
H14A H 0.1728 0.6685 -0.1395 0.031 Uiso 1 1 calc R . .
C15 C 0.2437(4) 0.5977(3) 0.0719(4) 0.0196(10) Uani 1 1 d . . .
C16 C 0.5377(4) 0.8491(3) 0.1469(4) 0.0223(10) Uani 1 1 d . . .
C17 C 0.3069(5) 0.3768(4) 0.7214(5) 0.0393(13) Uani 1 1 d . . .
H17A H 0.2694 0.3283 0.7374 0.047 Uiso 1 1 calc R . .
C18 C 0.4003(6) 0.5049(4) 0.7380(6) 0.0519(17) Uani 1 1 d . . .
H18A H 0.4370 0.5608 0.7676 0.062 Uiso 1 1 calc R . .
C19 C 0.3895(4) 0.4611(4) 0.6377(5) 0.0366(13) Uani 1 1 d . . .
H19A H 0.4178 0.4808 0.5860 0.044 Uiso 1 1 calc R . .
C20 C 0.2927(6) 0.3159(4) 0.5341(6) 0.0549(18) Uani 1 1 d . . .
H20A H 0.2514 0.2670 0.5490 0.082 Uiso 1 1 calc R . .
H20B H 0.3587 0.2909 0.5298 0.082 Uiso 1 1 calc R . .
H20C H 0.2440 0.3454 0.4603 0.082 Uiso 1 1 calc R . .
C21 C 0.3290(13) 0.4739(6) 0.8882(9) 0.131(5) Uani 1 1 d D . .
H21A H 0.3920 0.5128 0.9403 0.157 Uiso 1 1 calc R . .
H21B H 0.2598 0.5105 0.8606 0.157 Uiso 1 1 calc R . .
C22 C 0.3196(12) 0.4010(5) 0.9557(8) 0.115(4) Uani 1 1 d D . .
H22A H 0.3092 0.4252 1.0209 0.172 Uiso 1 1 calc R . .
H22B H 0.3881 0.3644 0.9856 0.172 Uiso 1 1 calc R . .
H22C H 0.2551 0.3633 0.9070 0.172 Uiso 1 1 calc R . .
N1 N 0.3290(4) 0.3827(3) 0.6291(4) 0.0331(10) Uani 1 1 d . . .
N2 N 0.3471(5) 0.4510(4) 0.7860(5) 0.0536(15) Uani 1 1 d . . .

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 0.0175(5) 0.0169(5) 0.0177(6) 0.0010(4) 0.0056(4) -0.0004(4)
Mn2 0.0188(4) 0.0178(4) 0.0215(4) 0.0010(3) 0.0073(3) 0.0004(3)
O1 0.0360(19) 0.033(2) 0.022(2) -0.0023(15) 0.0134(17) 0.0083(16)
O2 0.0246(17) 0.032(2) 0.030(2) 0.0024(15) 0.0103(16) 0.0146(15)
O3 0.0266(16) 0.0245(17) 0.023(2) -0.0007(14) 0.0089(15) 0.0030(14)
O4 0.0215(15) 0.0199(16) 0.0253(19) -0.0055(13) 0.0110(14) -0.0008(13)
O5 0.0231(17) 0.0311(19) 0.034(2) 0.0048(16) 0.0099(16) -0.0048(15)
O6 0.0253(17) 0.0235(17) 0.028(2) 0.0041(14) 0.0074(16) -0.0063(14)
O7 0.0204(16) 0.0314(18) 0.0217(19) -0.0030(15) 0.0052(14) -0.0100(14)
O8 0.0237(16) 0.0249(17) 0.030(2) 0.0029(15) 0.0107(16) -0.0047(14)
C1 0.027(2) 0.025(2) 0.023(3) -0.003(2) 0.011(2) -0.001(2)
C2 0.020(2) 0.022(2) 0.017(2) 0.0000(18) 0.0061(19) 0.0024(18)
C3 0.022(2) 0.018(2) 0.029(3) 0.001(2) 0.007(2) 0.0032(19)
C4 0.034(3) 0.028(3) 0.023(3) 0.001(2) 0.010(2) 0.011(2)
C5 0.051(3) 0.038(3) 0.020(3) 0.002(2) 0.010(3) 0.017(3)
C6 0.037(3) 0.033(3) 0.030(3) 0.001(2) 0.011(3) 0.014(2)
C7 0.028(2) 0.021(2) 0.024(3) -0.0009(19) 0.014(2) 0.001(2)
C8 0.026(2) 0.023(2) 0.027(3) -0.001(2) 0.016(2) -0.002(2)
C9 0.017(2) 0.022(2) 0.025(3) -0.0021(19) 0.010(2) -0.0026(18)
C10 0.021(2) 0.020(2) 0.015(2) 0.0029(18) 0.0048(19) 0.0006(18)
C11 0.016(2) 0.021(2) 0.029(3) -0.003(2) 0.009(2) -0.0013(19)
C12 0.028(2) 0.029(3) 0.024(3) 0.001(2) 0.014(2) -0.004(2)
C13 0.029(2) 0.033(3) 0.022(3) 0.007(2) 0.002(2) 0.000(2)
C14 0.023(2) 0.029(3) 0.022(3) 0.003(2) 0.007(2) -0.002(2)
C15 0.017(2) 0.017(2) 0.026(3) -0.0008(19) 0.010(2) -0.0021(18)
C16 0.021(2) 0.018(2) 0.030(3) 0.003(2) 0.013(2) 0.0053(19)
C17 0.050(3) 0.034(3) 0.043(4) -0.003(3) 0.029(3) -0.013(3)
C18 0.061(4) 0.042(4) 0.060(5) -0.010(3) 0.034(4) -0.027(3)
C19 0.034(3) 0.039(3) 0.036(3) 0.006(3) 0.015(3) -0.007(2)
C20 0.087(5) 0.051(4) 0.040(4) -0.009(3) 0.040(4) -0.021(4)
C21 0.257(15) 0.101(7) 0.106(9) -0.049(7) 0.145(11) -0.069(9)
C22 0.255(14) 0.059(5) 0.074(7) -0.023(5) 0.112(9) -0.044(7)
N1 0.043(2) 0.032(2) 0.023(2) 0.0022(19) 0.014(2) -0.001(2)
N2 0.090(4) 0.045(3) 0.045(3) -0.018(2) 0.048(3) -0.029(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 O5 2.141(3) . ?
Mn1 O5 2.141(3) 3_565 ?
Mn1 O1 2.190(3) . ?
Mn1 O1 2.190(3) 3_565 ?
Mn1 O4 2.225(3) 4_575 ?
Mn1 O4 2.225(3) 2_545 ?
Mn2 O2 2.080(3) . ?
Mn2 O6 2.096(3) . ?
Mn2 O8 2.143(3) 2_645 ?
Mn2 O3 2.281(3) 2_545 ?
Mn2 O4 2.286(3) 2_545 ?
Mn2 O7 2.456(3) 2_645 ?
Mn2 C8 2.618(5) 2_545 ?
Mn2 C16 2.622(5) 2_645 ?
O1 C7 1.252(6) . ?
O2 C7 1.265(6) . ?
O3 C8 1.244(6) . ?
O3 Mn2 2.281(3) 2 ?
O4 C8 1.278(6) . ?
O4 Mn1 2.225(3) 2 ?
O4 Mn2 2.286(3) 2 ?
O5 C15 1.240(5) . ?
O6 C15 1.278(6) . ?
O7 C16 1.239(6) . ?
O7 Mn2 2.456(3) 2_655 ?
O8 C16 1.283(5) . ?
O8 Mn2 2.143(3) 2_655 ?
C1 C6 1.386(7) . ?
C1 C2 1.386(6) . ?
C1 C7 1.509(6) . ?
C2 C3 1.400(6) . ?
C3 C4 1.391(7) . ?
C3 C8 1.500(6) . ?
C4 C5 1.405(7) . ?
C5 C6 1.377(7) . ?
C8 Mn2 2.618(5) 2 ?
C9 C14 1.384(7) . ?
C9 C10 1.402(6) . ?
C9 C15 1.501(6) . ?
C10 C11 1.395(6) . ?
C11 C12 1.402(7) . ?
C11 C16 1.502(6) . ?
C12 C13 1.382(7) . ?
C13 C14 1.392(7) . ?
C16 Mn2 2.622(5) 2_655 ?
C17 N2 1.309(7) . ?
C17 N1 1.325(7) . ?
C18 N2 1.358(7) . ?
C18 C19 1.367(9) . ?
C19 N1 1.362(7) . ?
C20 N1 1.445(7) . ?
C21 C22 1.398(8) . ?
C21 N2 1.452(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Mn1 O5 180.0 . 3_565 ?
O5 Mn1 O1 91.58(14) . . ?
O5 Mn1 O1 88.42(14) 3_565 . ?
O5 Mn1 O1 88.42(14) . 3_565 ?
O5 Mn1 O1 91.58(14) 3_565 3_565 ?
O1 Mn1 O1 180.00(16) . 3_565 ?
O5 Mn1 O4 91.73(12) . 4_575 ?
O5 Mn1 O4 88.27(12) 3_565 4_575 ?
O1 Mn1 O4 88.37(12) . 4_575 ?
O1 Mn1 O4 91.63(12) 3_565 4_575 ?
O5 Mn1 O4 88.27(12) . 2_545 ?
O5 Mn1 O4 91.73(12) 3_565 2_545 ?
O1 Mn1 O4 91.63(12) . 2_545 ?
O1 Mn1 O4 88.37(12) 3_565 2_545 ?
O4 Mn1 O4 180.00(10) 4_575 2_545 ?
O2 Mn2 O6 100.64(14) . . ?
O2 Mn2 O8 97.87(13) . 2_645 ?
O6 Mn2 O8 105.74(13) . 2_645 ?
O2 Mn2 O3 87.44(13) . 2_545 ?
O6 Mn2 O3 159.85(13) . 2_545 ?
O8 Mn2 O3 91.21(12) 2_645 2_545 ?
O2 Mn2 O4 96.78(12) . 2_545 ?
O6 Mn2 O4 102.85(12) . 2_545 ?
O8 Mn2 O4 144.68(12) 2_645 2_545 ?
O3 Mn2 O4 57.56(11) 2_545 2_545 ?
O2 Mn2 O7 150.56(13) . 2_645 ?
O6 Mn2 O7 100.94(12) . 2_645 ?
O8 Mn2 O7 56.91(12) 2_645 2_645 ?
O3 Mn2 O7 79.00(11) 2_545 2_645 ?
O4 Mn2 O7 97.70(11) 2_545 2_645 ?
O2 Mn2 C8 91.77(14) . 2_545 ?
O6 Mn2 C8 131.98(15) . 2_545 ?
O8 Mn2 C8 118.31(14) 2_645 2_545 ?
O3 Mn2 C8 28.35(13) 2_545 2_545 ?
O4 Mn2 C8 29.22(13) 2_545 2_545 ?
O7 Mn2 C8 88.52(13) 2_645 2_545 ?
O2 Mn2 C16 124.66(14) . 2_645 ?
O6 Mn2 C16 107.40(13) . 2_645 ?
O8 Mn2 C16 29.07(13) 2_645 2_645 ?
O3 Mn2 C16 82.14(13) 2_545 2_645 ?
O4 Mn2 C16 121.04(13) 2_545 2_645 ?
O7 Mn2 C16 28.01(12) 2_645 2_645 ?
C8 Mn2 C16 102.59(14) 2_545 2_645 ?
C7 O1 Mn1 142.3(3) . . ?
C7 O2 Mn2 127.1(3) . . ?
C8 O3 Mn2 91.1(3) . 2 ?
C8 O4 Mn1 136.7(3) . 2 ?
C8 O4 Mn2 90.0(3) . 2 ?
Mn1 O4 Mn2 105.79(13) 2 2 ?
C15 O5 Mn1 143.5(3) . . ?
C15 O6 Mn2 126.6(3) . . ?
C16 O7 Mn2 83.5(3) . 2_655 ?
C16 O8 Mn2 96.7(3) . 2_655 ?
C6 C1 C2 118.7(4) . . ?
C6 C1 C7 121.1(4) . . ?
C2 C1 C7 120.1(4) . . ?
C1 C2 C3 120.6(4) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 C8 120.9(4) . . ?
C2 C3 C8 118.7(4) . . ?
C3 C4 C5 118.6(5) . . ?
C6 C5 C4 120.3(5) . . ?
C5 C6 C1 121.4(5) . . ?
O1 C7 O2 125.5(4) . . ?
O1 C7 C1 118.8(4) . . ?
O2 C7 C1 115.6(4) . . ?
O3 C8 O4 121.4(4) . . ?
O3 C8 C3 117.8(4) . . ?
O4 C8 C3 120.8(4) . . ?
O3 C8 Mn2 60.6(2) . 2 ?
O4 C8 Mn2 60.8(2) . 2 ?
C3 C8 Mn2 178.3(4) . 2 ?
C14 C9 C10 119.1(4) . . ?
C14 C9 C15 118.6(4) . . ?
C10 C9 C15 122.3(4) . . ?
C11 C10 C9 120.3(4) . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 C16 121.3(4) . . ?
C12 C11 C16 119.3(4) . . ?
C13 C12 C11 120.4(4) . . ?
C12 C13 C14 119.6(5) . . ?
C9 C14 C13 121.1(5) . . ?
O5 C15 O6 125.0(4) . . ?
O5 C15 C9 117.5(4) . . ?
O6 C15 C9 117.5(4) . . ?
O7 C16 O8 122.3(4) . . ?
O7 C16 C11 120.8(4) . . ?
O8 C16 C11 117.0(4) . . ?
O7 C16 Mn2 68.5(2) . 2_655 ?
O8 C16 Mn2 54.3(2) . 2_655 ?
C11 C16 Mn2 168.8(3) . 2_655 ?
N2 C17 N1 108.1(5) . . ?
N2 C18 C19 106.8(5) . . ?
N1 C19 C18 105.9(5) . . ?
C22 C21 N2 117.7(8) . . ?
C17 N1 C19 109.5(5) . . ?
C17 N1 C20 124.6(5) . . ?
C19 N1 C20 125.9(5) . . ?
C17 N2 C18 109.6(5) . . ?
C17 N2 C21 124.2(6) . . ?
C18 N2 C21 126.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.130