# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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#
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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_c2c
_database_code_depnum_ccdc_archive 'CCDC 916007'
#TrackingRef 'cif-complex1.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H54 Mg2 N2 O19 P2'
_chemical_formula_weight         1121.53
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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   33.3495(12)
_cell_length_b                   10.5440(3)
_cell_length_c                   15.0994(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.703(2)
_cell_angle_gamma                90.00
_cell_volume                     5158.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4785
_cell_measurement_theta_min      2.5145
_cell_measurement_theta_max      28.028
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22195
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         28.34
_reflns_number_total             6418
_reflns_number_gt                4472
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_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^)+(0.0837P)^2^+10.2660P] 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         6418
_refine_ls_number_parameters     351
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1869
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Mg1 Mg 0.02696(3) 0.08839(9) 0.36761(6) 0.0142(2) Uani 1 1 d . . .
O1 O 0.07733(6) 0.20351(19) 0.40611(13) 0.0168(4) Uani 1 1 d . . .
O2 O 0.21037(8) 0.0139(3) 0.3770(2) 0.0463(8) Uani 1 1 d . . .
H2 H 0.2256 -0.0464 0.3692 0.070 Uiso 1 1 calc R . .
O3 O 0.25861(7) 0.1302(3) 0.33555(19) 0.0440(7) Uani 1 1 d . . .
O4 O 0.00449(6) 0.7983(2) 0.55693(13) 0.0176(4) Uani 1 1 d . . .
O5 O 0.03558(7) 0.6488(2) 0.65410(13) 0.0241(5) Uani 1 1 d . . .
O6 O 0.05991(6) 0.0264(2) 0.80397(13) 0.0197(5) Uani 1 1 d . . .
O7 O 0.02380(6) 0.0325(2) 0.65879(13) 0.0199(5) Uani 1 1 d . . .
O8 O 0.0000 0.2002(3) 0.2500 0.0158(6) Uani 1 2 d S . .
O9 O 0.04758(6) -0.0230(2) 0.48408(13) 0.0197(5) Uani 1 1 d . . .
P1 P 0.10010(2) 0.30622(7) 0.46518(5) 0.01396(18) Uani 1 1 d . . .
C1 C 0.14952(9) 0.3306(3) 0.43941(19) 0.0172(6) Uani 1 1 d . . .
C2 C 0.16880(9) 0.2244(3) 0.4141(2) 0.0205(7) Uani 1 1 d . . .
H2A H 0.1557 0.1440 0.4112 0.025 Uiso 1 1 calc R . .
C3 C 0.20703(9) 0.2346(3) 0.3931(2) 0.0247(7) Uani 1 1 d . . .
C4 C 0.22578(10) 0.3527(4) 0.3974(2) 0.0287(8) Uani 1 1 d . . .
H4 H 0.2518 0.3604 0.3823 0.034 Uiso 1 1 calc R . .
C5 C 0.20723(10) 0.4592(4) 0.4232(2) 0.0309(8) Uani 1 1 d . . .
H5 H 0.2206 0.5393 0.4269 0.037 Uiso 1 1 calc R . .
C6 C 0.16878(10) 0.4480(3) 0.4437(2) 0.0252(7) Uani 1 1 d . . .
H6 H 0.1557 0.5210 0.4607 0.030 Uiso 1 1 calc R . .
C7 C 0.22793(10) 0.1223(4) 0.3648(2) 0.0315(8) Uani 1 1 d . . .
C8 C 0.11013(9) 0.2658(3) 0.58435(18) 0.0148(6) Uani 1 1 d . . .
C9 C 0.14776(9) 0.2862(3) 0.6455(2) 0.0234(7) Uani 1 1 d . . .
H9 H 0.1691 0.3313 0.6270 0.028 Uiso 1 1 calc R . .
C10 C 0.07332(8) 0.4543(3) 0.44749(19) 0.0146(6) Uani 1 1 d . . .
C11 C 0.06450(9) 0.5061(3) 0.35999(19) 0.0195(6) Uani 1 1 d . . .
H11 H 0.0731 0.4634 0.3123 0.023 Uiso 1 1 calc R . .
C12 C 0.04334(9) 0.6189(3) 0.3427(2) 0.0197(6) Uani 1 1 d . . .
H12 H 0.0380 0.6549 0.2834 0.024 Uiso 1 1 calc R . .
C13 C 0.02978(9) 0.6803(3) 0.41150(19) 0.0166(6) Uani 1 1 d . . .
H13 H 0.0148 0.7574 0.3989 0.020 Uiso 1 1 calc R . .
C14 C 0.03813(8) 0.6292(3) 0.49895(18) 0.0147(6) Uani 1 1 d . . .
C15 C 0.06000(9) 0.5164(3) 0.51665(19) 0.0163(6) Uani 1 1 d . . .
H15 H 0.0659 0.4813 0.5763 0.020 Uiso 1 1 calc R . .
C16 C 0.02506(9) 0.6957(3) 0.57641(19) 0.0164(6) Uani 1 1 d . . .
C17 C 0.15415(10) 0.2401(4) 0.7344(2) 0.0300(8) Uani 1 1 d . . .
H17 H 0.1795 0.2562 0.7771 0.036 Uiso 1 1 calc R . .
C18 C 0.12351(9) 0.1707(3) 0.7607(2) 0.0233(7) Uani 1 1 d . . .
H18 H 0.1283 0.1379 0.8209 0.028 Uiso 1 1 calc R . .
C19 C 0.08589(9) 0.1489(3) 0.69926(19) 0.0150(6) Uani 1 1 d . . .
C20 C 0.07913(9) 0.1997(3) 0.61229(19) 0.0146(6) Uani 1 1 d . . .
H20 H 0.0530 0.1894 0.5712 0.018 Uiso 1 1 calc R . .
C21 C 0.05403(8) 0.0635(3) 0.72315(19) 0.0143(6) Uani 1 1 d . . .
C1S C 0.21000(13) 0.3405(4) 0.1535(3) 0.0435(10) Uani 1 1 d . . .
H1S H 0.2117 0.4028 0.1997 0.052 Uiso 1 1 calc R . .
C2S C 0.1685(2) 0.1902(6) 0.0498(4) 0.099(2) Uani 1 1 d . . .
H2S1 H 0.1834 0.2223 0.0051 0.119 Uiso 1 1 calc R . .
H2S2 H 0.1387 0.1863 0.0197 0.119 Uiso 1 1 calc R . .
C3S C 0.1838(3) 0.0601(7) 0.0812(7) 0.142(4) Uani 1 1 d . . .
H3S1 H 0.2112 0.0667 0.1228 0.213 Uiso 1 1 calc R . .
H3S2 H 0.1857 0.0085 0.0283 0.213 Uiso 1 1 calc R . .
H3S3 H 0.1647 0.0200 0.1128 0.213 Uiso 1 1 calc R . .
C4S C 0.14012(12) 0.2992(4) 0.1713(3) 0.0395(9) Uani 1 1 d . . .
H4S1 H 0.1187 0.3488 0.1286 0.047 Uiso 1 1 calc R . .
H4S2 H 0.1501 0.3514 0.2267 0.047 Uiso 1 1 calc R . .
C5S C 0.12067(13) 0.1808(4) 0.1974(3) 0.0478(11) Uani 1 1 d . . .
H5S1 H 0.1057 0.1370 0.1422 0.072 Uiso 1 1 calc R . .
H5S2 H 0.1014 0.2032 0.2349 0.072 Uiso 1 1 calc R . .
H5S3 H 0.1422 0.1249 0.2322 0.072 Uiso 1 1 calc R . .
N1S N 0.17496(11) 0.2763(4) 0.1283(2) 0.0481(9) Uani 1 1 d . . .
O1S O 0.24087(11) 0.3257(3) 0.1215(3) 0.0696(11) 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
Mg1 0.0188(5) 0.0102(5) 0.0162(5) -0.0002(4) 0.0090(4) -0.0003(4)
O1 0.0203(10) 0.0114(11) 0.0214(10) -0.0038(8) 0.0104(8) -0.0019(8)
O2 0.0320(14) 0.0359(17) 0.079(2) -0.0232(16) 0.0290(14) -0.0018(13)
O3 0.0274(13) 0.058(2) 0.0532(17) -0.0123(15) 0.0231(12) 0.0023(13)
O4 0.0220(10) 0.0144(11) 0.0196(10) 0.0013(8) 0.0118(8) 0.0039(9)
O5 0.0400(13) 0.0202(12) 0.0154(10) 0.0038(9) 0.0131(9) 0.0125(10)
O6 0.0245(11) 0.0163(12) 0.0199(10) 0.0056(9) 0.0082(8) -0.0010(9)
O7 0.0217(10) 0.0177(12) 0.0208(10) 0.0031(9) 0.0061(8) -0.0049(9)
O8 0.0225(14) 0.0099(15) 0.0175(14) 0.000 0.0099(11) 0.000
O9 0.0249(11) 0.0117(11) 0.0220(10) 0.0011(9) 0.0049(8) -0.0004(9)
P1 0.0189(4) 0.0090(4) 0.0170(4) -0.0003(3) 0.0103(3) -0.0012(3)
C1 0.0189(14) 0.0183(17) 0.0158(13) -0.0004(12) 0.0069(11) -0.0013(12)
C2 0.0205(15) 0.0192(17) 0.0244(15) -0.0032(13) 0.0106(12) -0.0044(13)
C3 0.0203(15) 0.032(2) 0.0240(16) -0.0027(14) 0.0100(13) -0.0004(14)
C4 0.0224(16) 0.038(2) 0.0287(17) 0.0016(16) 0.0120(13) -0.0054(15)
C5 0.0296(18) 0.026(2) 0.041(2) 0.0012(16) 0.0148(15) -0.0129(16)
C6 0.0275(16) 0.0196(18) 0.0307(17) -0.0003(14) 0.0113(13) -0.0048(14)
C7 0.0213(16) 0.041(2) 0.0339(18) -0.0112(17) 0.0093(14) 0.0001(16)
C8 0.0208(14) 0.0082(14) 0.0177(13) 0.0002(11) 0.0092(11) 0.0000(11)
C9 0.0222(15) 0.0234(19) 0.0255(16) 0.0040(14) 0.0073(12) -0.0067(14)
C10 0.0186(14) 0.0080(14) 0.0201(14) -0.0008(11) 0.0104(11) 0.0003(11)
C11 0.0289(16) 0.0145(16) 0.0173(14) -0.0024(12) 0.0101(12) -0.0004(13)
C12 0.0275(16) 0.0166(16) 0.0169(13) 0.0002(12) 0.0088(12) -0.0011(13)
C13 0.0235(15) 0.0089(15) 0.0185(14) 0.0012(11) 0.0073(11) -0.0013(12)
C14 0.0172(13) 0.0146(15) 0.0141(13) -0.0026(11) 0.0071(10) -0.0026(12)
C15 0.0214(14) 0.0120(15) 0.0169(13) -0.0011(11) 0.0073(11) -0.0013(12)
C16 0.0203(14) 0.0131(15) 0.0185(14) -0.0009(12) 0.0102(11) 0.0007(12)
C17 0.0234(16) 0.041(2) 0.0233(16) 0.0069(15) 0.0005(13) -0.0128(16)
C18 0.0256(16) 0.0260(19) 0.0178(14) 0.0067(13) 0.0040(12) -0.0051(14)
C19 0.0189(14) 0.0102(15) 0.0179(13) -0.0019(11) 0.0080(11) -0.0004(12)
C20 0.0175(13) 0.0108(15) 0.0172(13) -0.0012(11) 0.0074(11) 0.0003(11)
C21 0.0176(13) 0.0073(14) 0.0205(14) 0.0017(11) 0.0095(11) 0.0009(11)
C1S 0.045(2) 0.042(3) 0.047(2) 0.014(2) 0.0187(19) -0.004(2)
C2S 0.154(6) 0.075(5) 0.096(5) -0.037(4) 0.085(5) -0.061(4)
C3S 0.158(8) 0.064(5) 0.246(11) -0.040(6) 0.134(8) -0.009(5)
C4S 0.035(2) 0.036(2) 0.046(2) 0.0015(19) 0.0052(17) -0.0013(18)
C5S 0.045(2) 0.049(3) 0.050(2) 0.002(2) 0.013(2) -0.008(2)
N1S 0.059(2) 0.041(2) 0.053(2) -0.0088(17) 0.0296(18) -0.0155(18)
O1S 0.070(2) 0.046(2) 0.113(3) 0.014(2) 0.060(2) -0.0029(17)
_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
Mg1 O6 2.024(2) 6 ?
Mg1 O1 2.042(2) . ?
Mg1 O7 2.080(2) 5_556 ?
Mg1 O9 2.091(2) . ?
Mg1 O4 2.096(2) 5_566 ?
Mg1 O8 2.1439(18) . ?
Mg1 Mg1 3.5806(18) 2 ?
O1 P1 1.491(2) . ?
O2 C7 1.317(5) . ?
O3 C7 1.209(4) . ?
O4 C16 1.277(3) . ?
O4 Mg1 2.096(2) 5_566 ?
O5 C16 1.245(3) . ?
O6 C21 1.252(3) . ?
O6 Mg1 2.024(2) 6_556 ?
O7 C21 1.266(3) . ?
O7 Mg1 2.080(2) 5_556 ?
O8 Mg1 2.1439(18) 2 ?
P1 C10 1.788(3) . ?
P1 C1 1.799(3) . ?
P1 C8 1.802(3) . ?
C1 C6 1.389(4) . ?
C1 C2 1.389(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.388(5) . ?
C3 C7 1.487(5) . ?
C4 C5 1.382(5) . ?
C5 C6 1.394(4) . ?
C8 C9 1.388(4) . ?
C8 C20 1.392(4) . ?
C9 C17 1.396(4) . ?
C10 C15 1.391(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.376(4) . ?
C12 C13 1.387(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.388(4) . ?
C14 C16 1.513(4) . ?
C17 C18 1.389(4) . ?
C18 C19 1.391(4) . ?
C19 C20 1.386(4) . ?
C19 C21 1.500(4) . ?
C1S O1S 1.246(5) . ?
C1S N1S 1.326(5) . ?
C2S N1S 1.467(6) . ?
C2S C3S 1.502(10) . ?
C4S N1S 1.479(5) . ?
C4S C5S 1.502(6) . ?
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
O6 Mg1 O1 89.32(9) 6 . ?
O6 Mg1 O7 92.94(9) 6 5_556 ?
O1 Mg1 O7 174.66(9) . 5_556 ?
O6 Mg1 O9 87.47(9) 6 . ?
O1 Mg1 O9 90.57(9) . . ?
O7 Mg1 O9 84.70(9) 5_556 . ?
O6 Mg1 O4 175.57(10) 6 5_566 ?
O1 Mg1 O4 89.44(9) . 5_566 ?
O7 Mg1 O4 87.94(9) 5_556 5_566 ?
O9 Mg1 O4 88.29(9) . 5_566 ?
O6 Mg1 O8 95.97(8) 6 . ?
O1 Mg1 O8 93.67(8) . . ?
O7 Mg1 O8 90.90(8) 5_556 . ?
O9 Mg1 O8 174.56(7) . . ?
O4 Mg1 O8 88.34(8) 5_566 . ?
O6 Mg1 Mg1 74.37(6) 6 2 ?
O1 Mg1 Mg1 117.92(7) . 2 ?
O7 Mg1 Mg1 67.38(6) 5_556 2 ?
O9 Mg1 Mg1 145.29(6) . 2 ?
O4 Mg1 Mg1 109.93(7) 5_566 2 ?
O8 Mg1 Mg1 33.38(7) . 2 ?
P1 O1 Mg1 150.44(13) . . ?
C16 O4 Mg1 131.93(18) . 5_566 ?
C21 O6 Mg1 132.25(19) . 6_556 ?
C21 O7 Mg1 140.27(19) . 5_556 ?
Mg1 O8 Mg1 113.25(14) . 2 ?
O1 P1 C10 112.30(13) . . ?
O1 P1 C1 109.71(13) . . ?
C10 P1 C1 107.07(14) . . ?
O1 P1 C8 111.91(13) . . ?
C10 P1 C8 108.91(13) . . ?
C1 P1 C8 106.68(13) . . ?
C6 C1 C2 119.5(3) . . ?
C6 C1 P1 123.7(2) . . ?
C2 C1 P1 116.8(2) . . ?
C1 C2 C3 120.7(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 C7 119.4(3) . . ?
C2 C3 C7 121.5(3) . . ?
C5 C4 C3 121.0(3) . . ?
C4 C5 C6 119.4(3) . . ?
C1 C6 C5 120.3(3) . . ?
O3 C7 O2 123.6(4) . . ?
O3 C7 C3 123.0(4) . . ?
O2 C7 C3 113.4(3) . . ?
C9 C8 C20 119.7(3) . . ?
C9 C8 P1 123.5(2) . . ?
C20 C8 P1 116.5(2) . . ?
C8 C9 C17 119.6(3) . . ?
C15 C10 C11 119.6(3) . . ?
C15 C10 P1 122.4(2) . . ?
C11 C10 P1 118.0(2) . . ?
C12 C11 C10 120.1(3) . . ?
C11 C12 C13 120.4(3) . . ?
C12 C13 C14 120.1(3) . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 C16 118.9(2) . . ?
C13 C14 C16 121.6(3) . . ?
C14 C15 C10 120.3(3) . . ?
O5 C16 O4 124.7(3) . . ?
O5 C16 C14 118.4(3) . . ?
O4 C16 C14 116.8(2) . . ?
C18 C17 C9 120.2(3) . . ?
C17 C18 C19 120.3(3) . . ?
C20 C19 C18 119.1(3) . . ?
C20 C19 C21 119.6(3) . . ?
C18 C19 C21 121.1(3) . . ?
C19 C20 C8 121.0(3) . . ?
O6 C21 O7 125.4(3) . . ?
O6 C21 C19 117.7(2) . . ?
O7 C21 C19 116.8(2) . . ?
O1S C1S N1S 125.3(5) . . ?
N1S C2S C3S 109.7(6) . . ?
N1S C4S C5S 114.4(4) . . ?
C1S N1S C2S 119.9(4) . . ?
C1S N1S C4S 121.4(4) . . ?
C2S N1S C4S 118.3(4) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.506
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.149


data_squeezed
_database_code_depnum_ccdc_archive 'CCDC 916008'
#TrackingRef 'cif-complex2.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H50 Mn3 N2 O22 P2'
_chemical_formula_weight         1233.66
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a                   40.229(8)
_cell_length_b                   21.504(4)
_cell_length_c                   15.251(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.11(3)
_cell_angle_gamma                90.00
_cell_volume                     12389(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    86162
_cell_measurement_theta_min      0.458
_cell_measurement_theta_max      29.591
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5064
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_process_details   HKL3000-Scalepack
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.80000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'bending magnet beamline'
_diffrn_radiation_monochromator  'Pt coated Si double crystal'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43489
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         29.60
_reflns_number_total             11919
_reflns_number_gt                9073
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'PAL ADSC Quantum-210'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_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^)+(0.1409P)^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         11919
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1855
_refine_ls_wR_factor_gt          0.1783
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.001
_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 0.233891(12) 0.457933(19) 0.63991(3) 0.02973(14) Uani 1 1 d . . .
Mn2 Mn 0.281795(12) 0.45287(2) 0.88798(3) 0.03081(14) Uani 1 1 d . . .
Mn3 Mn 0.466863(13) 0.07050(2) 0.98155(4) 0.04210(16) Uani 1 1 d . . .
O1 O 0.23551(6) 0.48374(10) 0.34738(14) 0.0372(5) Uani 1 1 d . . .
O2 O 0.20300(6) 0.48571(10) 0.19544(15) 0.0427(5) Uani 1 1 d . . .
O3 O 0.25778(5) 0.39486(10) 0.76268(12) 0.0324(5) Uani 1 1 d . . .
O4 O 0.27593(6) 0.47362(10) 1.18653(15) 0.0398(5) Uani 1 1 d . . .
O5 O 0.31321(6) 0.48844(10) 1.33250(14) 0.0389(5) Uani 1 1 d . . .
O6 O 0.21778(8) 0.51484(10) 0.51219(15) 0.0524(6) Uani 1 1 d . . .
O7 O 0.18974(6) 0.39605(9) 0.58671(13) 0.0337(5) Uani 1 1 d . . .
O8 O 0.23576(6) 0.09617(9) 0.42753(14) 0.0340(5) Uani 1 1 d . . .
O9 O 0.30204(6) 0.51117(9) 1.01209(13) 0.0346(5) Uani 1 1 d . . .
O10 O 0.24728(6) 0.10622(10) 1.04434(14) 0.0407(5) Uani 1 1 d . . .
O11 O 0.27591(6) 0.17357(10) 1.15674(14) 0.0394(5) Uani 1 1 d . . .
O12 O 0.32715(6) 0.39255(9) 0.94629(14) 0.0356(5) Uani 1 1 d . . .
O13 O 0.21320(6) 0.17519(10) 0.33088(14) 0.0401(5) Uani 1 1 d . . .
O14 O 0.47297(7) 0.17365(12) 0.9882(2) 0.0676(8) Uani 1 1 d . . .
O15 O 0.42273(6) 0.13734(10) 0.98964(17) 0.0454(5) Uani 1 1 d . . .
O16 O 0.02262(7) 0.44278(12) 0.5296(2) 0.0606(7) Uani 1 1 d . . .
O17 O 0.46891(9) 0.06444(16) 0.8394(2) 0.0820(10) Uani 1 1 d . . .
O18 O 0.07138(7) 0.49635(10) 0.55451(19) 0.0494(6) Uani 1 1 d . . .
O19 O 0.47623(7) 0.04400(14) 1.12787(19) 0.0657(8) Uani 1 1 d . . .
P1 P 0.34203(2) 0.33842(3) 1.00937(5) 0.03175(19) Uani 1 1 d . . .
P2 P 0.16956(2) 0.34706(3) 0.52107(5) 0.03026(18) Uani 1 1 d . . .
C1 C 0.18786(8) 0.40178(13) 0.38317(19) 0.0314(6) Uani 1 1 d . . .
H1 H 0.2096 0.4098 0.4322 0.038 Uiso 1 1 calc R . .
C2 C 0.18265(8) 0.42433(13) 0.2932(2) 0.0337(6) Uani 1 1 d . . .
C3 C 0.15155(9) 0.40964(16) 0.2211(2) 0.0454(8) Uani 1 1 d . . .
H3 H 0.1479 0.4241 0.1596 0.054 Uiso 1 1 calc R . .
C4 C 0.12563(10) 0.37381(18) 0.2385(2) 0.0515(9) Uani 1 1 d . . .
H4 H 0.1048 0.3625 0.1886 0.062 Uiso 1 1 calc R . .
C5 C 0.20947(8) 0.46748(14) 0.2770(2) 0.0342(6) Uani 1 1 d . . .
C6 C 0.30361(8) 0.46191(13) 1.2532(2) 0.0332(7) Uani 1 1 d . . .
C7 C 0.32819(8) 0.41436(13) 1.2380(2) 0.0326(6) Uani 1 1 d . . .
C8 C 0.35553(10) 0.38864(17) 1.3119(2) 0.0483(9) Uani 1 1 d . . .
H8 H 0.3585 0.4000 1.3743 0.058 Uiso 1 1 calc R . .
C9 C 0.37846(10) 0.3465(2) 1.2945(2) 0.0597(11) Uani 1 1 d . . .
H9A H 0.3968 0.3286 1.3454 0.072 Uiso 1 1 calc R . .
C10 C 0.22120(8) 0.14939(13) 0.40833(19) 0.0311(6) Uani 1 1 d . . .
C11 C 0.19816(8) 0.24128(13) 0.4701(2) 0.0321(6) Uani 1 1 d . . .
H11 H 0.1927 0.2597 0.4102 0.039 Uiso 1 1 calc R . .
C12 C 0.21349(8) 0.18279(13) 0.48673(19) 0.0298(6) Uani 1 1 d . . .
C13 C 0.22162(8) 0.15527(14) 0.5743(2) 0.0336(6) Uani 1 1 d . . .
H13 H 0.2320 0.1150 0.5857 0.040 Uiso 1 1 calc R . .
C14 C 0.21438(8) 0.18742(14) 0.6448(2) 0.0337(6) Uani 1 1 d . . .
H14 H 0.2200 0.1688 0.7047 0.040 Uiso 1 1 calc R . .
C15 C 0.19920(8) 0.24587(14) 0.6295(2) 0.0335(6) Uani 1 1 d . . .
H15 H 0.1946 0.2675 0.6784 0.040 Uiso 1 1 calc R . .
C16 C 0.26682(8) 0.15333(13) 1.0749(2) 0.0325(6) Uani 1 1 d . . .
C17 C 0.28104(8) 0.18618(13) 1.0075(2) 0.0312(6) Uani 1 1 d . . .
C18 C 0.27297(8) 0.16498(14) 0.9159(2) 0.0347(7) Uani 1 1 d . . .
H18 H 0.2583 0.1295 0.8952 0.042 Uiso 1 1 calc R . .
C19 C 0.30225(8) 0.23849(13) 1.0370(2) 0.0324(6) Uani 1 1 d . . .
H19 H 0.3079 0.2530 1.0992 0.039 Uiso 1 1 calc R . .
C20 C 0.31520(8) 0.26966(13) 0.9756(2) 0.0320(6) Uani 1 1 d . . .
C21 C 0.30734(9) 0.24796(14) 0.8847(2) 0.0360(7) Uani 1 1 d . . .
H21 H 0.3164 0.2691 0.8431 0.043 Uiso 1 1 calc R . .
C22 C 0.28639(8) 0.19587(14) 0.8547(2) 0.0345(7) Uani 1 1 d . . .
H22 H 0.2811 0.1811 0.7927 0.041 Uiso 1 1 calc R . .
C23 C 0.32400(8) 0.39659(13) 1.1468(2) 0.0321(6) Uani 1 1 d . . .
H23 H 0.3048 0.4127 1.0961 0.039 Uiso 1 1 calc R . .
C24 C 0.34761(8) 0.35559(14) 1.1296(2) 0.0338(6) Uani 1 1 d . . .
C25 C 0.37503(10) 0.32986(18) 1.2036(2) 0.0499(9) Uani 1 1 d . . .
H25 H 0.3911 0.3014 1.1922 0.060 Uiso 1 1 calc R . .
C26 C 0.38523(8) 0.31879(14) 1.0074(2) 0.0347(7) Uani 1 1 d . . .
C27 C 0.39668(8) 0.25836(13) 1.0026(2) 0.0336(6) Uani 1 1 d . . .
H27 H 0.3813 0.2245 1.0005 0.040 Uiso 1 1 calc R . .
C28 C 0.43083(9) 0.24694(14) 1.0010(2) 0.0364(7) Uani 1 1 d . . .
C29 C 0.45357(9) 0.29667(15) 1.0067(3) 0.0456(8) Uani 1 1 d . . .
H29 H 0.4770 0.2892 1.0079 0.055 Uiso 1 1 calc R . .
C30 C 0.44210(10) 0.35749(16) 1.0108(3) 0.0511(9) Uani 1 1 d . . .
H30 H 0.4576 0.3914 1.0135 0.061 Uiso 1 1 calc R . .
C31 C 0.40839(10) 0.36836(15) 1.0107(2) 0.0447(8) Uani 1 1 d . . .
H31 H 0.4007 0.4099 1.0130 0.054 Uiso 1 1 calc R . .
C32 C 0.44302(9) 0.18179(15) 0.9934(2) 0.0408(7) Uani 1 1 d . . .
C33 C 0.05437(9) 0.44539(15) 0.5416(2) 0.0425(8) Uani 1 1 d . . .
C34 C 0.07400(8) 0.38730(14) 0.5367(2) 0.0367(7) Uani 1 1 d . . .
C35 C 0.10856(9) 0.39080(14) 0.5377(2) 0.0376(7) Uani 1 1 d . . .
H35 H 0.1200 0.4300 0.5439 0.045 Uiso 1 1 calc R . .
C36 C 0.12655(8) 0.33666(14) 0.5297(2) 0.0339(6) Uani 1 1 d . . .
C37 C 0.10990(9) 0.27931(15) 0.5205(2) 0.0412(7) Uani 1 1 d . . .
H37 H 0.1219 0.2426 0.5139 0.049 Uiso 1 1 calc R . .
C38 C 0.07520(9) 0.27604(15) 0.5210(3) 0.0483(8) Uani 1 1 d . . .
H38 H 0.0640 0.2367 0.5169 0.058 Uiso 1 1 calc R . .
C39 C 0.05707(9) 0.32926(14) 0.5274(2) 0.0427(8) Uani 1 1 d . . .
H39 H 0.0333 0.3267 0.5257 0.051 Uiso 1 1 calc R . .
C40 C 0.19069(8) 0.27302(14) 0.5402(2) 0.0331(6) Uani 1 1 d . . .
C41 C 0.16161(8) 0.36794(13) 0.4012(2) 0.0327(6) Uani 1 1 d . . .
C42 C 0.13033(9) 0.35467(16) 0.3286(2) 0.0443(8) Uani 1 1 d . . .
H42 H 0.1121 0.3323 0.3409 0.053 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
Mn1 0.0420(3) 0.0272(3) 0.0244(2) -0.00109(16) 0.01708(19) -0.00075(17)
Mn2 0.0439(3) 0.0285(3) 0.0248(2) -0.00046(16) 0.0180(2) -0.00125(18)
Mn3 0.0412(3) 0.0362(3) 0.0535(3) 0.0027(2) 0.0222(2) 0.0010(2)
O1 0.0448(12) 0.0341(12) 0.0355(11) 0.0038(9) 0.0172(10) -0.0037(9)
O2 0.0551(14) 0.0417(13) 0.0334(11) 0.0083(10) 0.0182(10) -0.0059(10)
O3 0.0461(12) 0.0316(11) 0.0229(10) -0.0010(8) 0.0160(9) -0.0010(9)
O4 0.0514(14) 0.0360(12) 0.0348(11) -0.0023(9) 0.0186(10) 0.0060(10)
O5 0.0529(13) 0.0396(13) 0.0284(10) -0.0068(9) 0.0193(10) 0.0001(10)
O6 0.0906(19) 0.0323(13) 0.0280(11) 0.0016(9) 0.0125(12) -0.0030(12)
O7 0.0425(12) 0.0323(11) 0.0297(10) -0.0026(8) 0.0166(9) -0.0056(9)
O8 0.0481(12) 0.0300(11) 0.0310(10) 0.0020(8) 0.0226(9) 0.0045(9)
O9 0.0512(13) 0.0297(11) 0.0273(10) -0.0028(8) 0.0193(9) 0.0000(9)
O10 0.0628(15) 0.0376(12) 0.0307(11) -0.0056(9) 0.0277(10) -0.0139(11)
O11 0.0593(14) 0.0367(12) 0.0279(11) -0.0023(9) 0.0223(10) -0.0090(10)
O12 0.0483(13) 0.0308(11) 0.0324(11) 0.0040(9) 0.0201(9) 0.0041(9)
O13 0.0633(15) 0.0354(12) 0.0288(11) 0.0040(9) 0.0248(10) 0.0069(10)
O14 0.0557(16) 0.0396(15) 0.120(3) 0.0132(15) 0.0460(17) 0.0120(12)
O15 0.0494(14) 0.0365(13) 0.0528(14) -0.0038(10) 0.0206(11) 0.0043(11)
O16 0.0419(14) 0.0451(15) 0.098(2) -0.0114(14) 0.0287(14) -0.0009(11)
O17 0.084(2) 0.116(3) 0.0513(17) 0.0013(17) 0.0301(16) -0.032(2)
O18 0.0516(14) 0.0330(13) 0.0686(16) -0.0025(11) 0.0273(13) 0.0012(10)
O19 0.0636(18) 0.079(2) 0.0540(17) 0.0126(14) 0.0200(14) 0.0049(14)
P1 0.0446(4) 0.0275(4) 0.0291(4) 0.0008(3) 0.0203(3) 0.0015(3)
P2 0.0386(4) 0.0295(4) 0.0280(4) -0.0007(3) 0.0183(3) -0.0015(3)
C1 0.0417(16) 0.0275(15) 0.0272(14) -0.0026(11) 0.0148(12) 0.0016(12)
C2 0.0441(17) 0.0277(16) 0.0323(15) 0.0030(12) 0.0170(13) 0.0036(12)
C3 0.053(2) 0.053(2) 0.0310(16) 0.0074(15) 0.0144(14) -0.0071(16)
C4 0.049(2) 0.067(2) 0.0360(18) 0.0054(16) 0.0120(15) -0.0127(17)
C5 0.0433(17) 0.0310(16) 0.0332(16) 0.0013(12) 0.0193(13) 0.0014(13)
C6 0.0463(18) 0.0293(16) 0.0293(15) 0.0021(12) 0.0198(13) 0.0014(12)
C7 0.0434(17) 0.0320(16) 0.0282(14) -0.0008(12) 0.0198(13) -0.0013(12)
C8 0.054(2) 0.065(2) 0.0288(16) -0.0005(15) 0.0178(15) 0.0135(17)
C9 0.056(2) 0.089(3) 0.0333(18) 0.0073(18) 0.0141(16) 0.031(2)
C10 0.0402(16) 0.0280(15) 0.0298(14) 0.0017(11) 0.0181(12) -0.0005(12)
C11 0.0373(16) 0.0335(16) 0.0293(14) 0.0000(12) 0.0161(12) -0.0022(12)
C12 0.0369(15) 0.0320(15) 0.0250(13) -0.0007(11) 0.0164(12) -0.0015(12)
C13 0.0423(17) 0.0326(16) 0.0300(15) 0.0007(12) 0.0176(13) -0.0001(12)
C14 0.0430(17) 0.0352(16) 0.0264(14) 0.0031(12) 0.0164(12) 0.0003(13)
C15 0.0439(17) 0.0320(16) 0.0294(14) -0.0012(12) 0.0188(13) -0.0024(13)
C16 0.0461(17) 0.0260(16) 0.0305(15) -0.0010(12) 0.0198(13) -0.0019(12)
C17 0.0388(16) 0.0282(15) 0.0326(15) 0.0013(12) 0.0200(12) 0.0004(12)
C18 0.0444(17) 0.0324(17) 0.0317(15) -0.0020(12) 0.0190(13) -0.0023(13)
C19 0.0398(16) 0.0315(16) 0.0299(14) -0.0004(12) 0.0173(12) 0.0032(12)
C20 0.0423(16) 0.0278(15) 0.0304(14) 0.0021(11) 0.0182(13) 0.0040(12)
C21 0.0494(18) 0.0333(17) 0.0317(15) 0.0041(12) 0.0220(14) 0.0032(13)
C22 0.0460(17) 0.0343(16) 0.0270(14) 0.0006(12) 0.0174(13) 0.0007(13)
C23 0.0425(17) 0.0280(15) 0.0279(14) 0.0004(11) 0.0147(12) 0.0003(12)
C24 0.0470(18) 0.0310(16) 0.0302(15) 0.0018(12) 0.0219(13) 0.0011(13)
C25 0.057(2) 0.062(2) 0.0356(17) 0.0065(16) 0.0215(16) 0.0217(17)
C26 0.0483(18) 0.0324(16) 0.0308(15) -0.0007(12) 0.0230(13) 0.0009(13)
C27 0.0420(17) 0.0278(16) 0.0340(15) 0.0039(12) 0.0171(13) 0.0004(12)
C28 0.0453(17) 0.0320(17) 0.0353(16) -0.0006(13) 0.0183(13) 0.0002(13)
C29 0.0432(18) 0.044(2) 0.056(2) -0.0004(16) 0.0252(16) 0.0023(15)
C30 0.050(2) 0.0375(19) 0.073(3) -0.0030(17) 0.0309(19) -0.0068(15)
C31 0.058(2) 0.0285(17) 0.054(2) -0.0011(14) 0.0273(17) -0.0008(14)
C32 0.0433(18) 0.0383(18) 0.0439(18) 0.0036(14) 0.0188(15) 0.0073(14)
C33 0.0424(19) 0.0379(19) 0.0490(19) -0.0011(15) 0.0181(15) 0.0014(14)
C34 0.0408(17) 0.0301(16) 0.0432(17) 0.0025(13) 0.0197(14) 0.0018(12)
C35 0.0472(18) 0.0289(16) 0.0389(16) -0.0008(13) 0.0176(14) -0.0023(13)
C36 0.0390(16) 0.0321(16) 0.0357(16) -0.0003(12) 0.0194(13) -0.0020(12)
C37 0.0428(18) 0.0308(17) 0.053(2) -0.0006(14) 0.0203(15) -0.0004(13)
C38 0.0471(19) 0.0314(18) 0.072(2) 0.0013(16) 0.0270(18) -0.0045(14)
C39 0.0406(18) 0.0363(18) 0.056(2) 0.0024(15) 0.0226(15) -0.0013(14)
C40 0.0392(16) 0.0340(16) 0.0301(14) -0.0033(12) 0.0169(12) -0.0041(12)
C41 0.0419(16) 0.0294(16) 0.0306(14) -0.0011(12) 0.0175(13) 0.0014(12)
C42 0.0452(19) 0.052(2) 0.0378(17) 0.0031(15) 0.0166(15) -0.0105(15)
_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 O2 2.111(2) 6_566 ?
Mn1 O7 2.143(2) . ?
Mn1 O4 2.169(2) 6_565 ?
Mn1 O8 2.183(2) 7_556 ?
Mn1 O6 2.201(2) . ?
Mn1 O3 2.243(2) . ?
Mn2 O5 2.154(2) 6_565 ?
Mn2 O12 2.165(2) . ?
Mn2 O9 2.181(2) . ?
Mn2 O3 2.207(2) . ?
Mn2 O10 2.209(2) 7_557 ?
Mn2 O1 2.217(2) 6_566 ?
Mn3 O16 2.126(3) 8_556 ?
Mn3 O18 2.152(2) 4_546 ?
Mn3 O17 2.201(3) . ?
Mn3 O19 2.206(3) . ?
Mn3 O14 2.230(3) . ?
Mn3 O15 2.320(2) . ?
Mn3 C32 2.607(3) . ?
O1 C5 1.264(4) . ?
O1 Mn2 2.217(2) 6_565 ?
O2 C5 1.244(4) . ?
O2 Mn1 2.111(2) 6_565 ?
O4 C6 1.248(4) . ?
O4 Mn1 2.169(2) 6_566 ?
O5 C6 1.271(4) . ?
O5 Mn2 2.154(2) 6_566 ?
O7 P2 1.487(2) . ?
O8 C10 1.273(3) . ?
O8 Mn1 2.183(2) 7_556 ?
O10 C16 1.269(4) . ?
O10 Mn2 2.209(2) 7_557 ?
O11 C16 1.251(3) . ?
O12 P1 1.498(2) . ?
O13 C10 1.243(3) . ?
O14 C32 1.246(4) . ?
O15 C32 1.245(4) . ?
O16 C33 1.227(4) . ?
O16 Mn3 2.126(3) 8_455 ?
O18 C33 1.271(4) . ?
O18 Mn3 2.152(2) 4_556 ?
P1 C20 1.798(3) . ?
P1 C26 1.799(3) . ?
P1 C24 1.807(3) . ?
P2 C40 1.781(3) . ?
P2 C36 1.794(3) . ?
P2 C41 1.801(3) . ?
C1 C41 1.386(4) . ?
C1 C2 1.401(4) . ?
C2 C3 1.389(5) . ?
C2 C5 1.506(4) . ?
C3 C4 1.393(5) . ?
C4 C42 1.384(5) . ?
C6 C7 1.495(4) . ?
C7 C8 1.390(5) . ?
C7 C23 1.397(4) . ?
C8 C9 1.383(5) . ?
C9 C25 1.392(5) . ?
C10 C12 1.516(4) . ?
C11 C12 1.385(4) . ?
C11 C40 1.386(4) . ?
C12 C13 1.393(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.382(4) . ?
C15 C40 1.412(4) . ?
C16 C17 1.513(4) . ?
C17 C19 1.390(4) . ?
C17 C18 1.398(4) . ?
C18 C22 1.396(4) . ?
C19 C20 1.390(4) . ?
C20 C21 1.392(4) . ?
C21 C22 1.382(4) . ?
C23 C24 1.385(4) . ?
C24 C25 1.393(5) . ?
C26 C27 1.389(4) . ?
C26 C31 1.405(5) . ?
C27 C28 1.404(4) . ?
C28 C29 1.390(5) . ?
C28 C32 1.502(4) . ?
C29 C30 1.395(5) . ?
C30 C31 1.376(5) . ?
C33 C34 1.494(4) . ?
C34 C35 1.387(4) . ?
C34 C39 1.405(4) . ?
C35 C36 1.398(4) . ?
C36 C37 1.387(4) . ?
C37 C38 1.400(5) . ?
C38 C39 1.379(5) . ?
C41 C42 1.391(4) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O7 89.01(9) 6_566 . ?
O2 Mn1 O4 88.80(9) 6_566 6_565 ?
O7 Mn1 O4 175.34(8) . 6_565 ?
O2 Mn1 O8 175.55(8) 6_566 7_556 ?
O7 Mn1 O8 90.89(8) . 7_556 ?
O4 Mn1 O8 90.97(8) 6_565 7_556 ?
O2 Mn1 O6 90.06(9) 6_566 . ?
O7 Mn1 O6 93.25(9) . . ?
O4 Mn1 O6 82.64(9) 6_565 . ?
O8 Mn1 O6 85.49(9) 7_556 . ?
O2 Mn1 O3 98.89(8) 6_566 . ?
O7 Mn1 O3 90.11(8) . . ?
O4 Mn1 O3 94.29(8) 6_565 . ?
O8 Mn1 O3 85.56(7) 7_556 . ?
O6 Mn1 O3 170.49(9) . . ?
O5 Mn2 O12 89.26(8) 6_565 . ?
O5 Mn2 O9 84.82(8) 6_565 . ?
O12 Mn2 O9 88.71(8) . . ?
O5 Mn2 O3 97.61(8) 6_565 . ?
O12 Mn2 O3 94.19(8) . . ?
O9 Mn2 O3 176.23(8) . . ?
O5 Mn2 O10 175.56(8) 6_565 7_557 ?
O12 Mn2 O10 88.30(8) . 7_557 ?
O9 Mn2 O10 91.42(8) . 7_557 ?
O3 Mn2 O10 86.27(8) . 7_557 ?
O5 Mn2 O1 94.58(8) 6_565 6_566 ?
O12 Mn2 O1 172.46(7) . 6_566 ?
O9 Mn2 O1 85.19(8) . 6_566 ?
O3 Mn2 O1 91.73(8) . 6_566 ?
O10 Mn2 O1 87.44(9) 7_557 6_566 ?
O16 Mn3 O18 124.43(10) 8_556 4_546 ?
O16 Mn3 O17 86.49(13) 8_556 . ?
O18 Mn3 O17 88.28(11) 4_546 . ?
O16 Mn3 O19 79.86(12) 8_556 . ?
O18 Mn3 O19 85.73(11) 4_546 . ?
O17 Mn3 O19 158.35(13) . . ?
O16 Mn3 O14 91.80(10) 8_556 . ?
O18 Mn3 O14 143.76(10) 4_546 . ?
O17 Mn3 O14 93.60(13) . . ?
O19 Mn3 O14 103.48(12) . . ?
O16 Mn3 O15 143.22(10) 8_556 . ?
O18 Mn3 O15 88.84(9) 4_546 . ?
O17 Mn3 O15 112.18(12) . . ?
O19 Mn3 O15 88.50(10) . . ?
O14 Mn3 O15 57.03(9) . . ?
O16 Mn3 C32 117.98(11) 8_556 . ?
O18 Mn3 C32 116.75(10) 4_546 . ?
O17 Mn3 C32 105.16(12) . . ?
O19 Mn3 C32 96.10(11) . . ?
O14 Mn3 C32 28.52(10) . . ?
O15 Mn3 C32 28.52(9) . . ?
C5 O1 Mn2 141.11(19) . 6_565 ?
C5 O2 Mn1 129.3(2) . 6_565 ?
Mn2 O3 Mn1 108.38(9) . . ?
C6 O4 Mn1 141.3(2) . 6_566 ?
C6 O5 Mn2 127.5(2) . 6_566 ?
P2 O7 Mn1 152.15(13) . . ?
C10 O8 Mn1 131.18(17) . 7_556 ?
C16 O10 Mn2 130.40(18) . 7_557 ?
P1 O12 Mn2 145.47(13) . . ?
C32 O14 Mn3 92.8(2) . . ?
C32 O15 Mn3 88.65(19) . . ?
C33 O16 Mn3 168.0(3) . 8_455 ?
C33 O18 Mn3 107.5(2) . 4_556 ?
O12 P1 C20 112.78(14) . . ?
O12 P1 C26 110.27(13) . . ?
C20 P1 C26 106.88(14) . . ?
O12 P1 C24 112.07(13) . . ?
C20 P1 C24 108.16(14) . . ?
C26 P1 C24 106.35(15) . . ?
O7 P2 C40 113.82(14) . . ?
O7 P2 C36 110.86(13) . . ?
C40 P2 C36 107.14(14) . . ?
O7 P2 C41 111.83(13) . . ?
C40 P2 C41 107.28(13) . . ?
C36 P2 C41 105.46(15) . . ?
C41 C1 C2 120.6(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C5 120.7(3) . . ?
C1 C2 C5 120.0(3) . . ?
C2 C3 C4 120.3(3) . . ?
C42 C4 C3 119.8(3) . . ?
O2 C5 O1 126.1(3) . . ?
O2 C5 C2 116.3(3) . . ?
O1 C5 C2 117.5(3) . . ?
O4 C6 O5 125.4(3) . . ?
O4 C6 C7 117.7(3) . . ?
O5 C6 C7 117.0(3) . . ?
C8 C7 C23 119.3(3) . . ?
C8 C7 C6 121.9(3) . . ?
C23 C7 C6 118.8(3) . . ?
C9 C8 C7 119.9(3) . . ?
C8 C9 C25 121.0(3) . . ?
O13 C10 O8 124.6(3) . . ?
O13 C10 C12 118.8(3) . . ?
O8 C10 C12 116.6(2) . . ?
C12 C11 C40 120.4(3) . . ?
C11 C12 C13 120.3(3) . . ?
C11 C12 C10 119.0(2) . . ?
C13 C12 C10 120.7(3) . . ?
C14 C13 C12 119.2(3) . . ?
C15 C14 C13 121.3(3) . . ?
C14 C15 C40 119.1(3) . . ?
O11 C16 O10 125.2(3) . . ?
O11 C16 C17 117.8(3) . . ?
O10 C16 C17 117.0(2) . . ?
C19 C17 C18 119.5(3) . . ?
C19 C17 C16 119.5(2) . . ?
C18 C17 C16 121.0(3) . . ?
C22 C18 C17 120.2(3) . . ?
C17 C19 C20 120.2(3) . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 P1 122.0(2) . . ?
C21 C20 P1 118.0(2) . . ?
C22 C21 C20 120.4(3) . . ?
C21 C22 C18 119.7(3) . . ?
C24 C23 C7 120.4(3) . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 P1 117.9(2) . . ?
C25 C24 P1 121.9(2) . . ?
C9 C25 C24 119.0(3) . . ?
C27 C26 C31 119.0(3) . . ?
C27 C26 P1 124.1(2) . . ?
C31 C26 P1 117.0(2) . . ?
C26 C27 C28 120.6(3) . . ?
C29 C28 C27 119.4(3) . . ?
C29 C28 C32 119.8(3) . . ?
C27 C28 C32 120.8(3) . . ?
C28 C29 C30 120.2(3) . . ?
C31 C30 C29 120.0(3) . . ?
C30 C31 C26 120.8(3) . . ?
O15 C32 O14 121.5(3) . . ?
O15 C32 C28 119.5(3) . . ?
O14 C32 C28 119.0(3) . . ?
O15 C32 Mn3 62.83(17) . . ?
O14 C32 Mn3 58.68(18) . . ?
C28 C32 Mn3 177.6(2) . . ?
O16 C33 O18 122.7(3) . . ?
O16 C33 C34 119.7(3) . . ?
O18 C33 C34 117.6(3) . . ?
C35 C34 C39 119.9(3) . . ?
C35 C34 C33 120.0(3) . . ?
C39 C34 C33 120.1(3) . . ?
C34 C35 C36 120.0(3) . . ?
C37 C36 C35 120.2(3) . . ?
C37 C36 P2 123.2(2) . . ?
C35 C36 P2 116.4(2) . . ?
C36 C37 C38 119.4(3) . . ?
C39 C38 C37 120.8(3) . . ?
C38 C39 C34 119.6(3) . . ?
C11 C40 C15 119.7(3) . . ?
C11 C40 P2 122.2(2) . . ?
C15 C40 P2 118.1(2) . . ?
C1 C41 C42 119.5(3) . . ?
C1 C41 P2 116.8(2) . . ?
C42 C41 P2 123.6(2) . . ?
C4 C42 C41 120.5(3) . . ?
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        29.60
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.729
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.113
# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.000 0.000 -0.007 2424.2 371.1
2 0.500 0.149 0.346 2424.3 371.1
_platon_squeeze_details          
;
The contributions of some 742 electrons were removed from the unit-cell contents, and as Z = 8 in this case,
this could/might correspond with the removal of solvent such as 2(DMF) and H2O [some 92 electrons]
per asymmetric unit.
;