# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_2
_database_code_depnum_ccdc_archive 'CCDC 864111'
#TrackingRef '14737_web_deposit_cif_file_0_Lin,Chu-Chieh_1350446940.complex 2 and 1a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H58 Ca Cl4 N8 O2'
_chemical_formula_sum            'C56 H58 Ca Cl4 N8 O2'
_chemical_formula_weight         1056.98

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'
Ca Ca 0.2262 0.3064 '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   'C 1 2/c 1'

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                   27.021(4)
_cell_length_b                   13.1464(12)
_cell_length_c                   17.215(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.30(2)
_cell_angle_gamma                90.00
_cell_volume                     5225.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5216
_cell_measurement_theta_min      2.7364
_cell_measurement_theta_max      27.2697

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2216
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.0690
_diffrn_reflns_number            10664
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         25.99
_reflns_number_total             5137
_reflns_number_gt                3829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1129P)^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         5137
_refine_ls_number_parameters     321
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1740
_refine_ls_wR_factor_gt          0.1667
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Ca Ca 0.5000 0.33306(5) 0.2500 0.0138(2) Uani 1 2 d S . .
O1 O 0.43528(7) 0.45380(13) 0.16581(12) 0.0174(4) Uani 1 1 d . . .
N2 N 0.29296(9) 0.54102(17) 0.07708(15) 0.0207(5) Uani 1 1 d . . .
N3 N 0.41500(9) 0.27863(16) 0.25685(14) 0.0177(5) Uani 1 1 d . . .
N1 N 0.34967(9) 0.54860(15) 0.09620(14) 0.0169(5) Uani 1 1 d . . .
N4 N 0.53561(9) 0.21442(16) 0.38856(14) 0.0182(5) Uani 1 1 d . . .
C17 C 0.21427(10) 0.13978(19) 0.17792(17) 0.0165(5) Uani 1 1 d . . .
C27 C 0.13770(11) 0.0041(2) 0.10804(17) 0.0207(6) Uani 1 1 d . . .
H27A H 0.1584 -0.0273 0.0854 0.025 Uiso 1 1 calc R . .
C4 C 0.36077(10) 0.30785(19) 0.20729(17) 0.0158(5) Uani 1 1 d . . .
C14 C 0.31202(10) 0.24620(19) 0.20068(17) 0.0172(5) Uani 1 1 d . . .
C22 C 0.16019(10) 0.09068(19) 0.16172(16) 0.0175(5) Uani 1 1 d . . .
C15 C 0.27954(11) 0.18333(19) 0.12618(17) 0.0184(5) Uani 1 1 d . . .
H15A H 0.2903 0.1759 0.0832 0.022 Uiso 1 1 calc R . .
C11 C 0.33997(14) 0.7996(2) -0.00662(19) 0.0284(7) Uani 1 1 d . . .
H11A H 0.3114 0.8454 -0.0450 0.034 Uiso 1 1 calc R . .
C23 C 0.12841(11) 0.1340(2) 0.19699(17) 0.0207(6) Uani 1 1 d . . .
H23A H 0.1429 0.1910 0.2341 0.025 Uiso 1 1 calc R . .
C2 C 0.28992(11) 0.45296(19) 0.11054(18) 0.0191(6) Uani 1 1 d . . .
C1 C 0.38245(11) 0.46452(18) 0.14286(16) 0.0155(5) Uani 1 1 d . . .
C24 C 0.07594(11) 0.0932(2) 0.17745(18) 0.0233(6) Uani 1 1 d . . .
H24A H 0.0556 0.1230 0.2015 0.028 Uiso 1 1 calc R . .
C7 C 0.36676(11) 0.64007(19) 0.07315(17) 0.0183(6) Uani 1 1 d . . .
C26 C 0.08470(12) -0.0364(2) 0.08776(19) 0.0256(6) Uani 1 1 d . . .
H26A H 0.0701 -0.0936 0.0509 0.031 Uiso 1 1 calc R . .
C12 C 0.32374(12) 0.7082(2) 0.01468(18) 0.0230(6) Uani 1 1 d . . .
H12A H 0.2848 0.6927 -0.0097 0.028 Uiso 1 1 calc R . .
C16 C 0.23176(11) 0.1317(2) 0.11453(17) 0.0189(5) Uani 1 1 d . . .
H16A H 0.2107 0.0908 0.0636 0.023 Uiso 1 1 calc R . .
C19 C 0.29640(11) 0.2525(2) 0.26666(17) 0.0216(6) Uani 1 1 d . . .
H19A H 0.3182 0.2921 0.3183 0.026 Uiso 1 1 calc R . .
C3 C 0.34453(10) 0.39980(19) 0.15358(17) 0.0162(5) Uani 1 1 d . . .
C18 C 0.24858(11) 0.1997(2) 0.25519(17) 0.0204(6) Uani 1 1 d . . .
H18A H 0.2390 0.2042 0.2998 0.024 Uiso 1 1 calc R . .
C9 C 0.43992(13) 0.7557(2) 0.0856(2) 0.0315(7) Uani 1 1 d . . .
H9A H 0.4787 0.7712 0.1087 0.038 Uiso 1 1 calc R . .
C25 C 0.05355(12) 0.0081(2) 0.12201(18) 0.0261(6) Uani 1 1 d . . .
H25A H 0.0180 -0.0188 0.1081 0.031 Uiso 1 1 calc R . .
C10 C 0.39757(14) 0.8238(2) 0.0280(2) 0.0290(7) Uani 1 1 d . . .
H10A H 0.4077 0.8850 0.0128 0.035 Uiso 1 1 calc R . .
C13 C 0.23309(11) 0.4271(2) 0.1025(2) 0.0299(7) Uani 1 1 d . . .
H13A H 0.2054 0.4796 0.0691 0.045 Uiso 1 1 calc R . .
H13B H 0.2386 0.4217 0.1622 0.045 Uiso 1 1 calc R . .
H13C H 0.2191 0.3635 0.0712 0.045 Uiso 1 1 calc R . .
C6 C 0.48655(11) 0.2057(2) 0.40323(17) 0.0197(6) Uani 1 1 d . . .
H6A H 0.4840 0.2676 0.4316 0.024 Uiso 1 1 calc R . .
H6B H 0.4939 0.1498 0.4447 0.024 Uiso 1 1 calc R . .
C5 C 0.42898(11) 0.1877(2) 0.31575(18) 0.0221(6) Uani 1 1 d . . .
H5A H 0.4315 0.1281 0.2848 0.026 Uiso 1 1 calc R . .
H5B H 0.3988 0.1764 0.3293 0.026 Uiso 1 1 calc R . .
C20 C 0.55509(12) 0.1123(2) 0.37947(19) 0.0262(6) Uani 1 1 d . . .
H20A H 0.5674 0.0740 0.4341 0.039 Uiso 1 1 calc R . .
H20B H 0.5868 0.1191 0.3696 0.039 Uiso 1 1 calc R . .
H20C H 0.5237 0.0775 0.3288 0.039 Uiso 1 1 calc R . .
C21 C 0.58456(12) 0.2662(2) 0.46592(18) 0.0288(7) Uani 1 1 d . . .
H21A H 0.5993 0.2246 0.5193 0.043 Uiso 1 1 calc R . .
H21B H 0.5718 0.3302 0.4762 0.043 Uiso 1 1 calc R . .
H21C H 0.6146 0.2777 0.4529 0.043 Uiso 1 1 calc R . .
C8 C 0.42519(12) 0.6643(2) 0.1094(2) 0.0249(6) Uani 1 1 d . . .
H8A H 0.4540 0.6197 0.1491 0.030 Uiso 1 1 calc R . .
Cl1 Cl 0.34831(6) 0.91117(8) 0.17307(7) 0.0698(4) Uani 1 1 d . . .
Cl2 Cl 0.41179(6) 0.93792(8) 0.36804(7) 0.0753(4) Uani 1 1 d . . .
C28 C 0.34269(15) 0.9432(3) 0.2666(2) 0.0389(8) Uani 1 1 d . . .
H28A H 0.3165 0.8964 0.2710 0.047 Uiso 1 1 calc R . .
H28B H 0.3269 1.0113 0.2587 0.047 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
Ca 0.0100(3) 0.0124(4) 0.0185(4) 0.000 0.0070(3) 0.000
O1 0.0124(9) 0.0166(9) 0.0242(9) 0.0040(7) 0.0101(8) 0.0019(7)
N2 0.0125(11) 0.0221(12) 0.0266(12) 0.0016(9) 0.0095(10) 0.0031(9)
N3 0.0145(10) 0.0168(11) 0.0213(11) 0.0051(9) 0.0091(9) 0.0006(9)
N1 0.0141(10) 0.0171(11) 0.0201(11) 0.0034(9) 0.0093(9) 0.0022(9)
N4 0.0141(11) 0.0165(11) 0.0211(11) 0.0022(9) 0.0071(9) 0.0005(9)
C17 0.0129(12) 0.0157(12) 0.0199(12) 0.0033(10) 0.0079(10) 0.0013(10)
C27 0.0200(13) 0.0223(14) 0.0209(13) 0.0012(11) 0.0114(11) -0.0019(11)
C4 0.0138(12) 0.0167(12) 0.0191(12) 0.0004(10) 0.0101(10) 0.0002(10)
C14 0.0133(12) 0.0165(12) 0.0217(13) 0.0046(10) 0.0091(10) 0.0019(10)
C22 0.0134(12) 0.0198(13) 0.0151(12) 0.0047(10) 0.0045(10) -0.0011(10)
C15 0.0185(13) 0.0198(13) 0.0196(13) 0.0005(11) 0.0118(11) 0.0010(11)
C11 0.0439(18) 0.0151(13) 0.0215(14) 0.0053(11) 0.0138(13) 0.0089(13)
C23 0.0174(13) 0.0227(14) 0.0204(13) -0.0001(11) 0.0087(11) -0.0023(11)
C2 0.0136(12) 0.0196(13) 0.0233(13) 0.0008(11) 0.0092(11) 0.0031(10)
C1 0.0158(12) 0.0145(12) 0.0159(12) 0.0012(10) 0.0080(10) 0.0032(10)
C24 0.0168(13) 0.0305(15) 0.0250(14) 0.0060(12) 0.0126(11) 0.0023(12)
C7 0.0242(14) 0.0139(12) 0.0199(13) 0.0012(10) 0.0136(11) 0.0012(11)
C26 0.0249(15) 0.0233(15) 0.0236(14) 0.0020(11) 0.0089(12) -0.0086(12)
C12 0.0245(14) 0.0192(13) 0.0220(14) 0.0016(11) 0.0097(12) 0.0054(11)
C16 0.0164(13) 0.0196(13) 0.0186(12) -0.0024(10) 0.0077(11) -0.0016(11)
C19 0.0180(13) 0.0266(14) 0.0185(13) -0.0039(11) 0.0084(11) -0.0054(11)
C3 0.0122(12) 0.0164(13) 0.0205(13) 0.0001(10) 0.0089(10) 0.0007(10)
C18 0.0168(13) 0.0263(14) 0.0215(13) -0.0002(11) 0.0125(11) -0.0026(11)
C9 0.0343(17) 0.0234(15) 0.0460(19) 0.0035(14) 0.0274(15) -0.0008(13)
C25 0.0165(13) 0.0322(16) 0.0251(14) 0.0057(12) 0.0078(11) -0.0086(12)
C10 0.0493(19) 0.0145(13) 0.0320(16) 0.0042(12) 0.0273(15) -0.0003(13)
C13 0.0146(13) 0.0264(15) 0.0477(18) 0.0073(14) 0.0156(13) 0.0045(12)
C6 0.0215(14) 0.0184(13) 0.0222(13) 0.0058(11) 0.0133(11) 0.0031(11)
C5 0.0154(13) 0.0223(14) 0.0292(14) 0.0085(12) 0.0120(12) 0.0013(11)
C20 0.0281(15) 0.0245(15) 0.0263(14) 0.0052(12) 0.0143(12) 0.0107(12)
C21 0.0229(15) 0.0304(16) 0.0207(14) 0.0031(12) 0.0026(12) -0.0065(12)
C8 0.0247(14) 0.0197(14) 0.0361(16) 0.0091(12) 0.0198(13) 0.0063(11)
Cl1 0.1118(10) 0.0606(7) 0.0483(6) -0.0031(5) 0.0495(6) 0.0084(6)
Cl2 0.1046(10) 0.0419(6) 0.0432(6) 0.0140(4) 0.0130(6) -0.0071(6)
C28 0.050(2) 0.0335(18) 0.0434(19) -0.0057(15) 0.0310(17) 0.0012(16)

_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
Ca O1 2.2460(18) 2_655 ?
Ca O1 2.2460(18) . ?
Ca N3 2.466(2) . ?
Ca N3 2.466(2) 2_655 ?
Ca N4 2.581(2) . ?
Ca N4 2.581(2) 2_655 ?
Ca C1 3.223(3) . ?
Ca C1 3.223(3) 2_655 ?
O1 C1 1.276(3) . ?
N2 C2 1.314(3) . ?
N2 N1 1.394(3) . ?
N3 C4 1.313(3) . ?
N3 C5 1.483(3) . ?
N1 C1 1.383(3) . ?
N1 C7 1.417(3) . ?
N4 C21 1.469(3) . ?
N4 C6 1.477(3) . ?
N4 C20 1.480(3) . ?
C17 C16 1.401(4) . ?
C17 C18 1.403(4) . ?
C17 C22 1.485(3) . ?
C27 C26 1.391(4) . ?
C27 C22 1.392(4) . ?
C27 H27A 0.9300 . ?
C4 C3 1.445(3) . ?
C4 C14 1.500(3) . ?
C14 C15 1.389(4) . ?
C14 C19 1.405(4) . ?
C22 C23 1.404(4) . ?
C15 C16 1.378(4) . ?
C15 H15A 0.9300 . ?
C11 C10 1.384(4) . ?
C11 C12 1.392(4) . ?
C11 H11A 0.9300 . ?
C23 C24 1.384(4) . ?
C23 H23A 0.9300 . ?
C2 C3 1.442(3) . ?
C2 C13 1.508(3) . ?
C1 C3 1.416(3) . ?
C24 C25 1.389(4) . ?
C24 H24A 0.9300 . ?
C7 C12 1.396(4) . ?
C7 C8 1.400(4) . ?
C26 C25 1.383(4) . ?
C26 H26A 0.9300 . ?
C12 H12A 0.9300 . ?
C16 H16A 0.9300 . ?
C19 C18 1.387(4) . ?
C19 H19A 0.9300 . ?
C18 H18A 0.9300 . ?
C9 C10 1.384(4) . ?
C9 C8 1.392(4) . ?
C9 H9A 0.9300 . ?
C25 H25A 0.9300 . ?
C10 H10A 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C6 C5 1.520(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C8 H8A 0.9300 . ?
Cl1 C28 1.745(3) . ?
Cl2 C28 1.776(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?

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 Ca O1 90.07(9) 2_655 . ?
O1 Ca N3 127.33(7) 2_655 . ?
O1 Ca N3 78.67(6) . . ?
O1 Ca N3 78.67(6) 2_655 2_655 ?
O1 Ca N3 127.33(7) . 2_655 ?
N3 Ca N3 146.27(10) . 2_655 ?
O1 Ca N4 92.25(7) 2_655 . ?
O1 Ca N4 144.56(6) . . ?
N3 Ca N4 71.93(7) . . ?
N3 Ca N4 87.68(7) 2_655 . ?
O1 Ca N4 144.56(6) 2_655 2_655 ?
O1 Ca N4 92.25(7) . 2_655 ?
N3 Ca N4 87.68(7) . 2_655 ?
N3 Ca N4 71.93(7) 2_655 2_655 ?
N4 Ca N4 105.65(10) . 2_655 ?
O1 Ca C1 101.29(7) 2_655 . ?
O1 Ca C1 17.53(6) . . ?
N3 Ca C1 61.16(7) . . ?
N3 Ca C1 142.51(7) 2_655 . ?
N4 Ca C1 129.50(7) . . ?
N4 Ca C1 90.67(7) 2_655 . ?
O1 Ca C1 17.53(6) 2_655 2_655 ?
O1 Ca C1 101.29(7) . 2_655 ?
N3 Ca C1 142.51(7) . 2_655 ?
N3 Ca C1 61.16(7) 2_655 2_655 ?
N4 Ca C1 90.68(7) . 2_655 ?
N4 Ca C1 129.50(7) 2_655 2_655 ?
C1 Ca C1 115.16(9) . 2_655 ?
C1 O1 Ca 130.45(15) . . ?
C2 N2 N1 105.7(2) . . ?
C4 N3 C5 118.8(2) . . ?
C4 N3 Ca 129.55(17) . . ?
C5 N3 Ca 110.72(15) . . ?
C1 N1 N2 111.96(19) . . ?
C1 N1 C7 129.6(2) . . ?
N2 N1 C7 118.2(2) . . ?
C21 N4 C6 110.3(2) . . ?
C21 N4 C20 108.3(2) . . ?
C6 N4 C20 110.3(2) . . ?
C21 N4 Ca 106.58(15) . . ?
C6 N4 Ca 105.56(14) . . ?
C20 N4 Ca 115.65(16) . . ?
C16 C17 C18 117.2(2) . . ?
C16 C17 C22 121.2(2) . . ?
C18 C17 C22 121.5(2) . . ?
C26 C27 C22 121.1(3) . . ?
C26 C27 H27A 119.4 . . ?
C22 C27 H27A 119.4 . . ?
N3 C4 C3 121.7(2) . . ?
N3 C4 C14 122.1(2) . . ?
C3 C4 C14 116.2(2) . . ?
C15 C14 C19 118.1(2) . . ?
C15 C14 C4 120.0(2) . . ?
C19 C14 C4 121.9(2) . . ?
C27 C22 C23 117.7(2) . . ?
C27 C22 C17 121.9(2) . . ?
C23 C22 C17 120.4(2) . . ?
C16 C15 C14 121.5(2) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C10 C11 C12 121.5(3) . . ?
C10 C11 H11A 119.2 . . ?
C12 C11 H11A 119.2 . . ?
C24 C23 C22 121.2(3) . . ?
C24 C23 H23A 119.4 . . ?
C22 C23 H23A 119.4 . . ?
N2 C2 C3 111.8(2) . . ?
N2 C2 C13 116.8(2) . . ?
C3 C2 C13 131.3(2) . . ?
O1 C1 N1 123.0(2) . . ?
O1 C1 C3 131.5(2) . . ?
N1 C1 C3 105.5(2) . . ?
O1 C1 Ca 32.02(11) . . ?
N1 C1 Ca 154.73(17) . . ?
C3 C1 Ca 99.67(15) . . ?
C23 C24 C25 120.3(3) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C12 C7 C8 119.9(2) . . ?
C12 C7 N1 118.4(2) . . ?
C8 C7 N1 121.7(2) . . ?
C25 C26 C27 120.4(3) . . ?
C25 C26 H26A 119.8 . . ?
C27 C26 H26A 119.8 . . ?
C11 C12 C7 119.0(3) . . ?
C11 C12 H12A 120.5 . . ?
C7 C12 H12A 120.5 . . ?
C15 C16 C17 121.3(2) . . ?
C15 C16 H16A 119.4 . . ?
C17 C16 H16A 119.4 . . ?
C18 C19 C14 120.3(2) . . ?
C18 C19 H19A 119.9 . . ?
C14 C19 H19A 119.8 . . ?
C1 C3 C2 105.0(2) . . ?
C1 C3 C4 125.9(2) . . ?
C2 C3 C4 128.6(2) . . ?
C19 C18 C17 121.6(2) . . ?
C19 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C26 C25 C24 119.3(2) . . ?
C26 C25 H25A 120.4 . . ?
C24 C25 H25A 120.4 . . ?
C9 C10 C11 119.1(3) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C6 C5 113.0(2) . . ?
N4 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N4 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N3 C5 C6 108.6(2) . . ?
N3 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N3 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
Cl1 C28 Cl2 110.29(19) . . ?
Cl1 C28 H28A 109.6 . . ?
Cl2 C28 H28A 109.6 . . ?
Cl1 C28 H28B 109.6 . . ?
Cl2 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.691
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.072


data_1a
_database_code_depnum_ccdc_archive 'CCDC 906296'
#TrackingRef '14737_web_deposit_cif_file_0_Lin,Chu-Chieh_1350446940.complex 2 and 1a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H16 Ca N4 O4'
_chemical_formula_sum            'C25 H16 Ca N4 O4'
_chemical_formula_weight         477.40

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'
Ca Ca 0.2262 0.3064 '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                   10.0497(10)
_cell_length_b                   16.055(3)
_cell_length_c                   19.540(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.412(12)
_cell_angle_gamma                90.00
_cell_volume                     3150.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    114(3)
_cell_measurement_reflns_used    1424
_cell_measurement_theta_min      2.6387
_cell_measurement_theta_max      29.1254

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             986
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      114(3)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.0690
_diffrn_reflns_number            16062
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_sigmaI/netI    0.2263
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6171
_reflns_number_gt                2509
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0728P)^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         6171
_refine_ls_number_parameters     327
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1743
_refine_ls_R_factor_gt           0.0987
_refine_ls_wR_factor_ref         0.2538
_refine_ls_wR_factor_gt          0.2263
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.029
_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
Ca Ca 0.43847(10) 0.90356(8) 0.02984(6) 0.0295(4) Uani 1 1 d . . .
O1 O 0.4805(3) 0.8855(3) 0.14235(18) 0.0344(11) Uani 1 1 d . . .
O2 O 0.3790(3) 1.0394(3) 0.02039(19) 0.0369(11) Uani 1 1 d . . .
O3 O 0.5968(4) 0.7963(3) 0.0007(2) 0.0409(11) Uani 1 1 d . . .
O4 O 0.8008(4) 0.7721(3) -0.0374(2) 0.0487(12) Uani 1 1 d . . .
N1 N 0.4392(4) 0.8698(3) 0.2587(2) 0.0277(11) Uani 1 1 d . . .
N2 N 0.3375(4) 0.8426(3) 0.2988(2) 0.0350(13) Uani 1 1 d . . .
N3 N 0.2331(4) 0.8280(3) 0.0635(2) 0.0280(11) Uani 1 1 d . . .
N4 N 0.3046(5) 0.8629(3) -0.0781(2) 0.0416(14) Uani 1 1 d U . .
C1 C 0.4035(5) 0.8642(4) 0.1897(3) 0.0295(14) Uani 1 1 d . . .
C2 C 0.2391(5) 0.8213(4) 0.2563(3) 0.0305(15) Uani 1 1 d . . .
C3 C 0.2724(5) 0.8328(3) 0.1867(3) 0.0242(13) Uani 1 1 d . . .
C4 C 0.1945(5) 0.8103(3) 0.1249(3) 0.0221(12) Uani 1 1 d . . .
C5 C 0.1498(5) 0.7948(5) 0.0045(3) 0.0396(17) Uani 1 1 d . . .
C6 C 0.1664(7) 0.8532(6) -0.0576(4) 0.053(3) Uani 0.888(14) 1 d P . .
C6' C 0.239(5) 0.787(4) -0.055(2) 0.053(3) Uani 0.134(13) 1 d P . .
C7 C 0.5599(5) 0.8971(3) 0.2919(3) 0.0264(13) Uani 1 1 d . . .
C8 C 0.6681(5) 0.9253(4) 0.2559(3) 0.0357(15) Uani 1 1 d . . .
H8A H 0.6634 0.9264 0.2083 0.043 Uiso 1 1 calc R . .
C9 C 0.7822(5) 0.9515(4) 0.2914(3) 0.0397(17) Uani 1 1 d . . .
H9A H 0.8536 0.9700 0.2668 0.048 Uiso 1 1 calc R . .
C10 C 0.7943(5) 0.9514(4) 0.3615(3) 0.0406(16) Uani 1 1 d . . .
H10A H 0.8717 0.9701 0.3843 0.049 Uiso 1 1 calc R . .
C11 C 0.6868(6) 0.9224(5) 0.3974(3) 0.0502(19) Uani 1 1 d . . .
H11A H 0.6916 0.9216 0.4451 0.060 Uiso 1 1 calc R . .
C12 C 0.5716(5) 0.8945(4) 0.3617(3) 0.0420(17) Uani 1 1 d . . .
H12A H 0.5014 0.8737 0.3861 0.050 Uiso 1 1 calc R . .
C13 C 0.1154(6) 0.7877(5) 0.2886(3) 0.0472(19) Uani 1 1 d . . .
H13A H 0.1282 0.7882 0.3376 0.071 Uiso 1 1 calc R . .
H13B H 0.0994 0.7317 0.2732 0.071 Uiso 1 1 calc R . .
H13C H 0.0403 0.8220 0.2755 0.071 Uiso 1 1 calc R . .
C14 C 0.0681(5) 0.7632(4) 0.1358(3) 0.0242(13) Uani 1 1 d . . .
C15 C 0.0709(5) 0.6771(4) 0.1423(3) 0.0343(15) Uani 1 1 d . . .
H15A H 0.1508 0.6488 0.1376 0.041 Uiso 1 1 calc R . .
C16 C -0.0433(6) 0.6325(4) 0.1557(3) 0.0392(16) Uani 1 1 d . . .
H16A H -0.0405 0.5749 0.1601 0.047 Uiso 1 1 calc R . .
C17 C -0.1611(6) 0.6752(4) 0.1624(3) 0.0350(15) Uani 1 1 d . . .
H17A H -0.2372 0.6460 0.1734 0.042 Uiso 1 1 calc R . .
C18 C -0.1684(5) 0.7593(4) 0.1531(3) 0.0414(17) Uani 1 1 d . . .
H18A H -0.2499 0.7865 0.1547 0.050 Uiso 1 1 calc R . .
C19 C -0.0522(5) 0.8045(4) 0.1413(3) 0.0299(14) Uani 1 1 d . . .
H19A H -0.0558 0.8622 0.1371 0.036 Uiso 1 1 calc R . .
C20 C 0.3497(8) 0.7762(6) -0.1082(4) 0.058(3) Uani 0.814(12) 1 d P . .
C20' C 0.401(3) 0.872(3) -0.1349(18) 0.058(3) Uani 0.208(12) 1 d P . .
C21 C 0.3157(9) 0.9248(6) -0.1312(4) 0.055(3) Uani 0.846(12) 1 d P . .
C21' C 0.197(4) 0.941(3) -0.089(2) 0.055(3) Uani 0.157(11) 1 d PU . .
C22 C 0.2391(11) 1.0731(7) 0.1138(6) 0.060(3) Uani 0.645(12) 1 d P . .
C22' C 0.1569(19) 1.0629(13) 0.0473(10) 0.060(3) Uani 0.379(11) 1 d P . .
C23 C 0.2807(6) 1.0884(4) 0.0465(4) 0.050(2) Uani 1 1 d . . .
C24 C 0.6988(5) 0.8214(4) -0.0244(3) 0.0354(16) Uani 1 1 d . . .
C25 C 0.7903(7) 0.6862(4) -0.0206(3) 0.0497(19) Uani 1 1 d . . .
H25A H 0.8699 0.6577 -0.0327 0.074 Uiso 1 1 calc R . .
H25B H 0.7150 0.6624 -0.0454 0.074 Uiso 1 1 calc R . .
H25C H 0.7787 0.6804 0.0277 0.074 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
Ca 0.0205(5) 0.0376(8) 0.0308(7) 0.0052(6) 0.0059(4) -0.0034(6)
O1 0.0228(18) 0.053(3) 0.028(2) 0.005(2) 0.0074(16) -0.0186(19)
O2 0.0228(18) 0.045(3) 0.043(3) 0.008(2) 0.0091(17) 0.0041(19)
O3 0.031(2) 0.041(3) 0.051(3) -0.005(2) 0.0041(19) -0.004(2)
O4 0.038(2) 0.042(3) 0.068(3) 0.005(3) 0.022(2) 0.003(2)
N1 0.027(2) 0.034(3) 0.021(3) -0.001(2) -0.0037(19) -0.005(2)
N2 0.023(2) 0.052(4) 0.030(3) 0.005(3) 0.003(2) -0.012(2)
N3 0.024(2) 0.036(3) 0.024(3) 0.003(2) 0.0044(18) -0.010(2)
N4 0.040(3) 0.056(4) 0.028(3) 0.003(3) -0.004(2) -0.016(3)
C1 0.022(3) 0.037(4) 0.030(3) 0.001(3) 0.000(2) -0.003(3)
C2 0.031(3) 0.045(4) 0.016(3) 0.010(3) 0.009(2) -0.004(3)
C3 0.017(2) 0.025(3) 0.031(3) 0.004(3) 0.005(2) 0.003(2)
C4 0.023(3) 0.021(3) 0.023(3) 0.000(2) 0.005(2) 0.001(2)
C5 0.033(3) 0.073(5) 0.012(3) 0.001(3) -0.011(2) -0.008(3)
C6 0.041(4) 0.091(8) 0.027(4) 0.007(5) 0.005(3) -0.023(5)
C6' 0.041(4) 0.091(8) 0.027(4) 0.007(5) 0.005(3) -0.023(5)
C7 0.024(3) 0.018(3) 0.037(4) 0.000(3) -0.005(2) -0.001(3)
C8 0.040(3) 0.035(4) 0.033(4) -0.012(3) 0.004(3) -0.001(3)
C9 0.014(2) 0.039(4) 0.066(5) -0.011(4) -0.008(3) -0.005(3)
C10 0.030(3) 0.034(4) 0.057(5) -0.007(3) -0.020(3) -0.003(3)
C11 0.056(4) 0.063(5) 0.031(4) 0.015(4) -0.010(3) -0.015(4)
C12 0.035(3) 0.055(5) 0.034(4) 0.016(3) -0.014(3) -0.007(3)
C13 0.041(3) 0.078(5) 0.023(4) -0.006(3) 0.011(3) -0.021(4)
C14 0.021(3) 0.030(4) 0.022(3) 0.007(3) 0.007(2) -0.001(3)
C15 0.028(3) 0.030(4) 0.044(4) 0.002(3) -0.001(3) -0.007(3)
C16 0.043(4) 0.030(4) 0.045(4) 0.004(3) 0.004(3) -0.010(3)
C17 0.032(3) 0.041(4) 0.032(4) 0.000(3) 0.004(3) -0.013(3)
C18 0.017(3) 0.054(5) 0.054(4) -0.007(4) 0.005(3) 0.004(3)
C19 0.033(3) 0.021(3) 0.036(4) -0.009(3) 0.007(2) -0.008(3)
C20 0.045(5) 0.076(7) 0.053(6) -0.036(5) -0.002(4) 0.006(5)
C20' 0.045(5) 0.076(7) 0.053(6) -0.036(5) -0.002(4) 0.006(5)
C21 0.071(6) 0.068(6) 0.024(4) 0.008(4) 0.003(4) -0.028(5)
C21' 0.071(6) 0.068(6) 0.024(4) 0.008(4) 0.003(4) -0.028(5)
C22 0.061(6) 0.056(7) 0.065(7) 0.000(6) 0.023(5) -0.006(6)
C22' 0.061(6) 0.056(7) 0.065(7) 0.000(6) 0.023(5) -0.006(6)
C23 0.035(3) 0.032(4) 0.087(5) 0.008(4) 0.040(3) 0.005(3)
C24 0.027(3) 0.052(5) 0.028(3) -0.005(3) -0.001(2) 0.003(3)
C25 0.056(4) 0.045(5) 0.049(4) -0.015(4) 0.011(3) 0.012(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
Ca O1 2.240(4) . ?
Ca O2 2.267(4) . ?
Ca O2 2.306(3) 3_675 ?
Ca O3 2.428(4) . ?
Ca N3 2.506(4) . ?
Ca N4 2.538(5) . ?
Ca C6' 3.16(5) . ?
Ca C24 3.153(6) . ?
Ca C1 3.220(6) . ?
Ca Ca 3.550(2) 3_675 ?
O1 C1 1.276(6) . ?
O2 C23 1.378(6) . ?
O2 Ca 2.306(3) 3_675 ?
O3 C24 1.224(6) . ?
O4 C24 1.328(7) . ?
O4 C25 1.423(7) . ?
N1 N2 1.384(6) . ?
N1 C1 1.384(7) . ?
N1 C7 1.421(6) . ?
N2 C2 1.309(7) . ?
N3 C4 1.306(6) . ?
N3 C5 1.494(7) . ?
N4 C21 1.444(9) . ?
N4 C6' 1.47(6) . ?
N4 C20' 1.51(3) . ?
N4 C6 1.470(8) . ?
N4 C20 1.585(10) . ?
N4 C21' 1.67(5) . ?
C1 C3 1.409(7) . ?
C2 C3 1.428(7) . ?
C2 C13 1.517(7) . ?
C3 C4 1.457(7) . ?
C4 C14 1.502(7) . ?
C5 C6' 1.49(5) . ?
C5 C6 1.549(10) . ?
C6 C6' 1.28(7) . ?
C6 C21' 1.58(5) . ?
C6' C20 1.57(5) . ?
C7 C12 1.364(8) . ?
C7 C8 1.395(7) . ?
C8 C9 1.380(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.370(8) . ?
C9 H9A 0.9300 . ?
C10 C11 1.393(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.401(8) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C19 1.388(7) . ?
C14 C15 1.388(8) . ?
C15 C16 1.387(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.378(8) . ?
C16 H16A 0.9300 . ?
C17 C18 1.364(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.402(7) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
C20 C20' 1.70(4) . ?
C20' C21 1.21(4) . ?
C21 C21' 1.51(4) . ?
C22 C23 1.418(12) . ?
C22 C22' 1.52(2) . ?
C22' C23 1.310(19) . ?
C23 C24 1.528(9) 3_675 ?
C24 C23 1.528(9) 3_675 ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 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
O1 Ca O2 104.05(15) . . ?
O1 Ca O2 110.41(13) . 3_675 ?
O2 Ca O2 78.16(14) . 3_675 ?
O1 Ca O3 92.27(15) . . ?
O2 Ca O3 146.75(14) . . ?
O2 Ca O3 68.97(14) 3_675 . ?
O1 Ca N3 78.61(13) . . ?
O2 Ca N3 105.68(14) . . ?
O2 Ca N3 169.34(15) 3_675 . ?
O3 Ca N3 105.84(15) . . ?
O1 Ca N4 148.60(15) . . ?
O2 Ca N4 92.92(17) . . ?
O2 Ca N4 98.71(15) 3_675 . ?
O3 Ca N4 87.29(16) . . ?
N3 Ca N4 71.37(15) . . ?
O1 Ca C6' 121.7(9) . . ?
O2 Ca C6' 111.5(13) . . ?
O2 Ca C6' 120.8(8) 3_675 . ?
O3 Ca C6' 82.4(12) . . ?
N3 Ca C6' 48.5(8) . . ?
N4 Ca C6' 27.2(10) . . ?
O1 Ca C24 98.66(14) . . ?
O2 Ca C24 126.49(15) . . ?
O2 Ca C24 48.46(16) 3_675 . ?
O3 Ca C24 20.53(15) . . ?
N3 Ca C24 126.16(17) . . ?
N4 Ca C24 91.82(16) . . ?
C6' Ca C24 95.5(11) . . ?
O1 Ca C1 17.52(12) . . ?
O2 Ca C1 103.21(14) . . ?
O2 Ca C1 127.73(14) 3_675 . ?
O3 Ca C1 100.79(15) . . ?
N3 Ca C1 61.67(14) . . ?
N4 Ca C1 132.83(15) . . ?
C6' Ca C1 107.3(8) . . ?
C24 Ca C1 111.69(15) . . ?
O1 Ca Ca 112.43(12) . 3_675 ?
O2 Ca Ca 39.47(9) . 3_675 ?
O2 Ca Ca 38.69(10) 3_675 3_675 ?
O3 Ca Ca 107.52(11) . 3_675 ?
N3 Ca Ca 144.19(12) . 3_675 ?
N4 Ca Ca 97.53(13) . 3_675 ?
C6' Ca Ca 124.5(10) . 3_675 ?
C24 Ca Ca 87.08(13) . 3_675 ?
C1 Ca Ca 122.92(12) . 3_675 ?
C1 O1 Ca 130.6(3) . . ?
C23 O2 Ca 135.2(4) . . ?
C23 O2 Ca 121.8(4) . 3_675 ?
Ca O2 Ca 101.83(14) . 3_675 ?
C24 O3 Ca 115.4(4) . . ?
C24 O4 C25 117.9(5) . . ?
N2 N1 C1 111.4(4) . . ?
N2 N1 C7 118.4(4) . . ?
C1 N1 C7 130.3(4) . . ?
C2 N2 N1 106.2(4) . . ?
C4 N3 C5 116.9(4) . . ?
C4 N3 Ca 128.8(4) . . ?
C5 N3 Ca 114.3(3) . . ?
C21 N4 C6' 148(2) . . ?
C21 N4 C20' 48.4(15) . . ?
C6' N4 C20' 128(3) . . ?
C21 N4 C6 111.8(6) . . ?
C6' N4 C6 52(2) . . ?
C20' N4 C6 148.4(13) . . ?
C21 N4 C20 107.8(6) . . ?
C6' N4 C20 62(2) . . ?
C20' N4 C20 66.8(16) . . ?
C6 N4 C20 107.2(6) . . ?
C21 N4 C21' 57.4(13) . . ?
C6' N4 C21' 111(3) . . ?
C20' N4 C21' 106(2) . . ?
C6 N4 C21' 59.8(14) . . ?
C20 N4 C21' 144.3(15) . . ?
C21 N4 Ca 111.5(4) . . ?
C6' N4 Ca 100.6(19) . . ?
C20' N4 Ca 104.7(12) . . ?
C6 N4 Ca 105.9(4) . . ?
C20 N4 Ca 112.6(4) . . ?
C21' N4 Ca 103.1(15) . . ?
O1 C1 N1 123.3(5) . . ?
O1 C1 C3 131.3(5) . . ?
N1 C1 C3 105.5(4) . . ?
O1 C1 Ca 31.9(2) . . ?
N1 C1 Ca 153.9(3) . . ?
C3 C1 Ca 99.8(3) . . ?
N2 C2 C3 111.7(5) . . ?
N2 C2 C13 116.1(5) . . ?
C3 C2 C13 132.2(5) . . ?
C1 C3 C2 105.3(5) . . ?
C1 C3 C4 126.3(4) . . ?
C2 C3 C4 128.2(5) . . ?
N3 C4 C3 122.4(4) . . ?
N3 C4 C14 121.7(5) . . ?
C3 C4 C14 115.8(4) . . ?
N3 C5 C6' 107.0(19) . . ?
N3 C5 C6 108.3(5) . . ?
C6' C5 C6 50(3) . . ?
C6' C6 N4 64(2) . . ?
C6' C6 C5 63(2) . . ?
N4 C6 C5 114.3(6) . . ?
C6' C6 C21' 130(3) . . ?
N4 C6 C21' 66.4(17) . . ?
C5 C6 C21' 151.0(17) . . ?
C6 C6' N4 64(3) . . ?
C6 C6' C5 67(3) . . ?
N4 C6' C5 118(5) . . ?
C6 C6' C20 119(4) . . ?
N4 C6' C20 62.7(17) . . ?
C5 C6' C20 171(4) . . ?
C6 C6' Ca 83(3) . . ?
N4 C6' Ca 52.3(16) . . ?
C5 C6' Ca 86(2) . . ?
C20 C6' Ca 87.8(19) . . ?
C12 C7 C8 118.5(5) . . ?
C12 C7 N1 118.9(5) . . ?
C8 C7 N1 122.6(5) . . ?
C9 C8 C7 119.6(6) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 122.6(6) . . ?
C10 C9 H9A 118.7 . . ?
C8 C9 H9A 118.7 . . ?
C9 C10 C11 117.8(5) . . ?
C9 C10 H10A 121.1 . . ?
C11 C10 H10A 121.1 . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C7 C12 C11 121.6(6) . . ?
C7 C12 H12A 119.2 . . ?
C11 C12 H12A 119.2 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 118.9(5) . . ?
C19 C14 C4 121.0(5) . . ?
C15 C14 C4 120.1(5) . . ?
C16 C15 C14 121.1(6) . . ?
C16 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
C17 C16 C15 118.9(6) . . ?
C17 C16 H16A 120.6 . . ?
C15 C16 H16A 120.6 . . ?
C16 C17 C18 121.4(5) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C17 C18 C19 119.6(5) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C14 C19 C18 120.0(5) . . ?
C14 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C6' C20 N4 55(2) . . ?
C6' C20 C20' 110(3) . . ?
N4 C20 C20' 54.5(11) . . ?
C21 C20' N4 63.0(15) . . ?
C21 C20' C20 113(2) . . ?
N4 C20' C20 58.7(15) . . ?
C20' C21 N4 68.6(19) . . ?
C20' C21 C21' 137(3) . . ?
N4 C21 C21' 68.8(18) . . ?
C21 C21' C6 103(3) . . ?
C21 C21' N4 53.8(17) . . ?
C6 C21' N4 53.8(16) . . ?
C23 C22 C22' 52.9(8) . . ?
C23 C22' C22 59.6(10) . . ?
C22' C23 O2 121.5(10) . . ?
C22' C23 C22 67.5(10) . . ?
O2 C23 C22 119.3(7) . . ?
C22' C23 C24 116.0(11) . 3_675 ?
O2 C23 C24 109.2(4) . 3_675 ?
C22 C23 C24 118.4(7) . 3_675 ?
O3 C24 O4 123.2(6) . . ?
O3 C24 C23 123.4(5) . 3_675 ?
O4 C24 C23 113.4(5) . 3_675 ?
O3 C24 Ca 44.1(3) . . ?
O4 C24 Ca 166.3(4) . . ?
C23 C24 Ca 79.8(3) 3_675 . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.093
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.024 0.000 0.496 485 122 ' '
2 -0.024 0.500 0.041 485 126 ' '
_platon_squeeze_details          
;
;