# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_1
_database_code_depnum_ccdc_archive 'CCDC 1024405'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_audit_creation_date             2015-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         '2(Br), C21 H28 Ca N4 O6, 3(H2 O)'
_chemical_formula_sum            'C21 H34 Br2 Ca N4 O9'
_chemical_formula_weight         686.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2450(6)
_cell_length_b                   11.6571(9)
_cell_length_c                   15.3212(13)
_cell_angle_alpha                100.778(7)
_cell_angle_beta                 99.668(7)
_cell_angle_gamma                91.324(6)
_cell_volume                     1423.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3430
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.84
_cell_measurement_theta_min      3.87
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.652
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4714
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.844
_diffrn_reflns_theta_min         3.866
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4291
_reflns_number_total             5338
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0575P)²+1.7772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1345
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O8A(0.65) H8AA(0.65) H8AB(0.65) O8B(0.35) H8BA(0.35) H8BB(0.35)
3.a Free rotating group:
 O7(H7A,H7B,O8A,H8AA,H8AB,O8B,H8BA,H8BB,O9,H9A,H9B)
3.b Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6C,H6D), C16(H16A,H16B), C20(H20A,H20B)
3.d Me refined with riding coordinates:
 C14(H14A,H14B,H14C)
3.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C17(H17), C18(H18), C19(H19)
3.f Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.13796(7) 0.39760(6) 0.83084(4) 0.05215(18) Uani 1 1 d . . . . .
Br2 Br 0.46458(6) 0.88230(4) 0.75138(3) 0.03934(15) Uani 1 1 d . . . . .
Ca1 Ca 0.25306(10) 0.44736(7) 0.46586(5) 0.0294(2) Uani 1 1 d . . . . .
O1 O 0.2499(4) 0.6520(3) 0.5040(2) 0.0390(7) Uani 1 1 d . . . . .
O2 O -0.0064(4) 0.6531(3) 0.5340(2) 0.0355(7) Uani 1 1 d . . . . .
O3 O 0.5104(4) 0.4784(3) 0.58805(19) 0.0340(7) Uani 1 1 d . . . . .
O4 O 0.2680(4) 0.4721(3) 0.6323(2) 0.0383(7) Uani 1 1 d . . . . .
O5 O 0.4113(4) 0.2809(3) 0.4294(2) 0.0409(8) Uani 1 1 d . . . . .
H5A H 0.4111 0.2235 0.3775 0.061 Uiso 1 1 d GR . . A 1
H5B H 0.5255 0.3019 0.4526 0.061 Uiso 1 1 d GR . . A 1
O6 O 0.0657(4) 0.4771(3) 0.3344(2) 0.0378(7) Uani 1 1 d . . . . .
H6A H 0.1163 0.5152 0.3029 0.057 Uiso 1 1 d GR . . . .
H6B H -0.0274 0.4877 0.3336 0.057 Uiso 1 1 d GR . . B 1
O7 O 0.3623(5) 0.7631(3) 0.3548(2) 0.0622(11) Uani 1 1 d . . . . .
H7A H 0.4587 0.7719 0.3434 0.093 Uiso 1 1 d G . . . .
H7B H 0.3658 0.7132 0.3917 0.093 Uiso 1 1 d G . . C 1
O8A O 0.3740(4) 1.1502(4) 0.7012(3) 0.121(4) Uani 0.65 1 d G . P D 1
H8AA H 0.3713 1.0771 0.6808 0.182 Uiso 0.65 1 d G . P E 1
H8AB H 0.4020 1.1632 0.7583 0.182 Uiso 0.65 1 d G . P F 1
O8B O 0.3600(4) 1.1081(4) 0.6500(3) 0.048(3) Uani 0.35 1 d G . P G 2
H8BA H 0.3405 1.0586 0.6006 0.071 Uiso 0.35 1 d G . P H 2
H8BB H 0.3869 1.0726 0.6935 0.071 Uiso 0.35 1 d G . P I 2
O9 O 0.0544(4) 1.2040(3) 0.6734(3) 0.0742(13) Uani 1 1 d G . . . .
H9A H 0.0315 1.2748 0.6894 0.111 Uiso 1 1 d G . . . .
H9B H 0.1528 1.2015 0.6639 0.111 Uiso 1 1 d G . . . .
N1 N 0.0209(4) 0.8939(3) 0.5895(2) 0.0308(8) Uani 1 1 d . . . . .
N2 N -0.0820(4) 0.9699(3) 0.7064(2) 0.0313(8) Uani 1 1 d . . . . .
N3 N 0.4062(4) 0.5536(3) 0.8110(2) 0.0309(8) Uani 1 1 d . . . . .
N4 N 0.2333(4) 0.6096(3) 0.8994(2) 0.0295(7) Uani 1 1 d . . . . .
C1 C 0.1237(5) 0.7025(4) 0.5249(3) 0.0316(9) Uani 1 1 d . . . . .
C2 C 0.1366(5) 0.8343(4) 0.5359(3) 0.0317(9) Uani 1 1 d . . . . .
H2A H 0.2480 0.8625 0.5645 0.038 Uiso 1 1 calc R . . . .
H2B H 0.1168 0.8547 0.4766 0.038 Uiso 1 1 calc R . . . .
C3 C -0.1374(5) 0.9202(4) 0.5583(3) 0.0342(10) Uani 1 1 d . . . . .
H3 H -0.1905 0.9069 0.4985 0.041 Uiso 1 1 calc R . . . .
C4 C -0.2013(5) 0.9693(4) 0.6318(3) 0.0339(10) Uani 1 1 d . . . . .
H4 H -0.3060 0.9973 0.6317 0.041 Uiso 1 1 calc R . . . .
C5 C 0.0508(5) 0.9240(4) 0.6790(3) 0.0328(9) Uani 1 1 d . . . . .
H5 H 0.1488 0.9144 0.7163 0.039 Uiso 1 1 calc R . . . .
C6 C -0.0974(5) 1.0169(4) 0.8013(3) 0.0336(9) Uani 1 1 d . . . . .
H6C H -0.2076 0.9970 0.8103 0.040 Uiso 1 1 calc R . . . .
H6D H -0.0824 1.1015 0.8130 0.040 Uiso 1 1 calc R . . . .
C7 C 0.0276(5) 0.9691(4) 0.8681(3) 0.0319(9) Uani 1 1 d . . . . .
C8 C 0.1544(5) 1.0433(4) 0.9240(3) 0.0319(9) Uani 1 1 d . . . . .
C9 C 0.2637(5) 0.9964(4) 0.9867(3) 0.0326(9) Uani 1 1 d . . . . .
H9 H 0.3469 1.0457 1.0250 0.039 Uiso 1 1 calc R . . . .
C10 C 0.2536(5) 0.8805(4) 0.9942(3) 0.0309(9) Uani 1 1 d . . . . .
C11 C 0.1256(5) 0.8069(4) 0.9373(3) 0.0318(9) Uani 1 1 d . . . . .
C12 C 0.0123(5) 0.8506(4) 0.8747(3) 0.0308(9) Uani 1 1 d . . . . .
C13 C 0.3779(6) 0.8351(5) 1.0623(3) 0.0384(11) Uani 1 1 d . . . . .
C14 C 0.1776(6) 1.1701(4) 0.9189(3) 0.0380(10) Uani 1 1 d . . . . .
H14A H 0.2710 1.2052 0.9628 0.057 Uiso 1 1 calc R . . . .
H14B H 0.1958 1.1761 0.8596 0.057 Uiso 1 1 calc R . . . .
H14C H 0.0807 1.2098 0.9311 0.057 Uiso 1 1 calc R . . . .
C15 C -0.1257(6) 0.7714(4) 0.8152(3) 0.0413(11) Uani 1 1 d . . . . .
H15A H -0.1977 0.8164 0.7805 0.062 Uiso 1 1 calc GR . . . .
H15B H -0.1866 0.7353 0.8520 0.062 Uiso 1 1 calc GR . . . .
H15C H -0.0807 0.7121 0.7752 0.062 Uiso 1 1 calc GR . . . .
C16 C 0.1135(5) 0.6805(4) 0.9465(3) 0.0335(9) Uani 1 1 d . . . . .
H16A H 0.1348 0.6761 1.0100 0.040 Uiso 1 1 calc R . . . .
H16B H 0.0025 0.6479 0.9213 0.040 Uiso 1 1 calc R . . . .
C17 C 0.3118(5) 0.6396(4) 0.8374(3) 0.0313(9) Uani 1 1 d . . . . .
H17 H 0.3023 0.7092 0.8160 0.038 Uiso 1 1 calc R . . . .
C18 C 0.2780(6) 0.5010(4) 0.9120(3) 0.0430(11) Uani 1 1 d . . . . .
H18 H 0.2411 0.4593 0.9517 0.052 Uiso 1 1 calc R . . . .
C19 C 0.3852(7) 0.4652(5) 0.8566(3) 0.0453(12) Uani 1 1 d . . . . .
H19 H 0.4354 0.3941 0.8504 0.054 Uiso 1 1 calc R . . . .
C20 C 0.5081(5) 0.5519(4) 0.7413(3) 0.0344(10) Uani 1 1 d . . . . .
H20A H 0.6057 0.5099 0.7566 0.041 Uiso 1 1 calc R . . . .
H20B H 0.5438 0.6316 0.7407 0.041 Uiso 1 1 calc R . . . .
C21 C 0.4192(5) 0.4952(4) 0.6474(3) 0.0313(9) Uani 1 1 d . . . . .
H13A H 0.432(6) 0.775(5) 1.031(4) 0.043(14) Uiso 1 1 d . . . . .
H13B H 0.326(6) 0.794(5) 1.103(4) 0.043(14) Uiso 1 1 d . . . . .
H13C H 0.437(6) 0.887(5) 1.091(3) 0.037(14) Uiso 1 1 d . . . . .


_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
Ca1 Ca1 4.1280(17) 2_666 ?
Ca1 O1 2.349(3) . ?
Ca1 O2 2.324(3) 2_566 ?
Ca1 O3 2.552(3) . ?
Ca1 O3 2.442(3) 2_666 ?
Ca1 O4 2.493(3) . ?
Ca1 O5 2.396(3) . ?
Ca1 O6 2.409(3) . ?
Ca1 C1 3.205(5) . ?
Ca1 C21 2.833(4) . ?
O1 C1 1.266(5) . ?
O2 Ca1 2.324(3) 2_566 ?
O2 C1 1.246(5) . ?
O3 Ca1 2.442(3) 2_666 ?
O3 C21 1.265(5) . ?
O4 C21 1.243(5) . ?
O5 H5A 0.9386 . ?
O5 H5B 0.9572 . ?
O6 H6A 0.8622 . ?
O6 H6B 0.7787 . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8820 . ?
O8A H8AA 0.8499 . ?
O8A H8AB 0.8499 . ?
O8B H8BA 0.8502 . ?
O8B H8BB 0.8497 . ?
O9 H9A 0.8505 . ?
O9 H9B 0.8491 . ?
N1 C2 1.465(5) . ?
N1 C3 1.375(6) . ?
N1 C5 1.329(6) . ?
N2 C4 1.376(5) . ?
N2 C5 1.326(6) . ?
N2 C6 1.483(5) . ?
N3 C17 1.329(6) . ?
N3 C19 1.372(6) . ?
N3 C20 1.463(5) . ?
N4 C16 1.495(5) . ?
N4 C17 1.328(5) . ?
N4 C18 1.366(6) . ?
C1 C2 1.513(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.358(6) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C6 C7 1.518(6) . ?
C7 C8 1.398(6) . ?
C7 C12 1.408(6) . ?
C8 C9 1.401(6) . ?
C8 C14 1.504(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.380(6) . ?
C10 C11 1.407(6) . ?
C10 C13 1.514(7) . ?
C11 C12 1.399(6) . ?
C11 C16 1.508(6) . ?
C12 C15 1.505(6) . ?
C13 H13A 0.93(6) . ?
C13 H13B 1.00(5) . ?
C13 H13C 0.78(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.346(7) . ?
C19 H19 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.521(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
O1 Ca1 Ca1 76.81(8) . 2_666 ?
O1 Ca1 O3 74.82(11) . 2_666 ?
O1 Ca1 O3 83.20(11) . . ?
O1 Ca1 O4 80.19(12) . . ?
O1 Ca1 O5 147.24(11) . . ?
O1 Ca1 O6 82.07(12) . . ?
O1 Ca1 C1 19.59(10) . . ?
O1 Ca1 C21 77.68(12) . . ?
O2 Ca1 Ca1 159.15(9) 2_566 2_666 ?
O2 Ca1 O1 114.92(12) 2_566 . ?
O2 Ca1 O3 160.58(11) 2_566 2_666 ?
O2 Ca1 O3 127.51(11) 2_566 . ?
O2 Ca1 O4 81.42(11) 2_566 . ?
O2 Ca1 O5 97.76(11) 2_566 . ?
O2 Ca1 O6 73.65(11) 2_566 . ?
O2 Ca1 C1 95.34(11) 2_566 . ?
O2 Ca1 C21 105.96(12) 2_566 . ?
O3 Ca1 Ca1 33.41(6) . 2_666 ?
O3 Ca1 Ca1 35.13(7) 2_666 2_666 ?
O3 Ca1 O3 68.54(11) 2_666 . ?
O3 Ca1 O4 117.57(10) 2_666 . ?
O3 Ca1 C1 93.66(11) 2_666 . ?
O3 Ca1 C1 95.04(10) . . ?
O3 Ca1 C21 92.32(11) 2_666 . ?
O3 Ca1 C21 26.51(11) . . ?
O4 Ca1 Ca1 83.95(7) . 2_666 ?
O4 Ca1 O3 52.18(9) . . ?
O4 Ca1 C1 75.47(11) . . ?
O4 Ca1 C21 26.00(11) . . ?
O5 Ca1 Ca1 71.40(8) . 2_666 ?
O5 Ca1 O3 74.71(11) . 2_666 ?
O5 Ca1 O3 74.72(11) . . ?
O5 Ca1 O4 103.73(12) . . ?
O5 Ca1 O6 110.74(12) . . ?
O5 Ca1 C1 166.61(11) . . ?
O5 Ca1 C21 91.82(12) . . ?
O6 Ca1 Ca1 126.51(8) . 2_666 ?
O6 Ca1 O3 158.17(11) . . ?
O6 Ca1 O3 92.03(11) . 2_666 ?
O6 Ca1 O4 139.52(11) . . ?
O6 Ca1 C1 75.69(11) . . ?
O6 Ca1 C21 157.37(13) . . ?
C1 Ca1 Ca1 95.28(8) . 2_666 ?
C21 Ca1 Ca1 58.04(9) . 2_666 ?
C21 Ca1 C1 81.88(12) . . ?
C1 O1 Ca1 122.0(3) . . ?
C1 O2 Ca1 173.8(3) . 2_566 ?
Ca1 O3 Ca1 111.46(11) 2_666 . ?
C21 O3 Ca1 146.0(3) . 2_666 ?
C21 O3 Ca1 89.2(3) . . ?
C21 O4 Ca1 92.4(2) . . ?
Ca1 O5 H5A 134.4 . . ?
Ca1 O5 H5B 109.2 . . ?
H5A O5 H5B 104.7 . . ?
Ca1 O6 H6A 110.0 . . ?
Ca1 O6 H6B 124.0 . . ?
H6A O6 H6B 116.7 . . ?
H7A O7 H7B 107.8 . . ?
H8AA O8A H8AB 109.4 . . ?
H8BA O8B H8BB 109.4 . . ?
H9A O9 H9B 109.6 . . ?
C3 N1 C2 127.0(4) . . ?
C5 N1 C2 124.1(4) . . ?
C5 N1 C3 108.8(4) . . ?
C4 N2 C6 125.8(4) . . ?
C5 N2 C4 108.5(4) . . ?
C5 N2 C6 125.7(4) . . ?
C17 N3 C19 108.6(4) . . ?
C17 N3 C20 125.2(4) . . ?
C19 N3 C20 126.2(4) . . ?
C17 N4 C16 126.4(4) . . ?
C17 N4 C18 108.4(4) . . ?
C18 N4 C16 125.3(4) . . ?
O1 C1 Ca1 38.5(2) . . ?
O1 C1 C2 114.6(4) . . ?
O2 C1 Ca1 87.4(3) . . ?
O2 C1 O1 125.8(4) . . ?
O2 C1 C2 119.6(4) . . ?
C2 C1 Ca1 152.5(3) . . ?
N1 C2 C1 113.7(3) . . ?
N1 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 H3 126.6 . . ?
C4 C3 N1 106.7(4) . . ?
C4 C3 H3 126.6 . . ?
N2 C4 H4 126.4 . . ?
C3 C4 N2 107.2(4) . . ?
C3 C4 H4 126.4 . . ?
N1 C5 H5 125.6 . . ?
N2 C5 N1 108.9(4) . . ?
N2 C5 H5 125.6 . . ?
N2 C6 H6C 109.2 . . ?
N2 C6 H6D 109.2 . . ?
N2 C6 C7 112.2(3) . . ?
H6C C6 H6D 107.9 . . ?
C7 C6 H6C 109.2 . . ?
C7 C6 H6D 109.2 . . ?
C8 C7 C6 120.0(4) . . ?
C8 C7 C12 120.5(4) . . ?
C12 C7 C6 119.5(4) . . ?
C7 C8 C9 118.1(4) . . ?
C7 C8 C14 122.6(4) . . ?
C9 C8 C14 119.3(4) . . ?
C8 C9 H9 118.5 . . ?
C10 C9 C8 122.9(4) . . ?
C10 C9 H9 118.5 . . ?
C9 C10 C11 118.3(4) . . ?
C9 C10 C13 120.2(4) . . ?
C11 C10 C13 121.5(4) . . ?
C10 C11 C16 118.2(4) . . ?
C12 C11 C10 120.6(4) . . ?
C12 C11 C16 121.3(4) . . ?
C7 C12 C15 120.3(4) . . ?
C11 C12 C7 119.6(4) . . ?
C11 C12 C15 120.0(4) . . ?
C10 C13 H13A 108(3) . . ?
C10 C13 H13B 113(3) . . ?
C10 C13 H13C 109(4) . . ?
H13A C13 H13B 102(4) . . ?
H13A C13 H13C 114(5) . . ?
H13B C13 H13C 110(5) . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 C11 111.8(3) . . ?
N4 C16 H16A 109.3 . . ?
N4 C16 H16B 109.3 . . ?
C11 C16 H16A 109.3 . . ?
C11 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
N3 C17 H17 125.7 . . ?
N4 C17 N3 108.6(4) . . ?
N4 C17 H17 125.7 . . ?
N4 C18 H18 126.2 . . ?
C19 C18 N4 107.7(4) . . ?
C19 C18 H18 126.2 . . ?
N3 C19 H19 126.6 . . ?
C18 C19 N3 106.8(4) . . ?
C18 C19 H19 126.6 . . ?
N3 C20 H20A 108.9 . . ?
N3 C20 H20B 108.9 . . ?
N3 C20 C21 113.3(3) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
O3 C21 Ca1 64.3(2) . . ?
O3 C21 C20 114.6(4) . . ?
O4 C21 Ca1 61.6(2) . . ?
O4 C21 O3 124.5(4) . . ?
O4 C21 C20 120.9(4) . . ?
C20 C21 Ca1 165.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O1 C1 O2 5.2(6) . . . . ?
Ca1 O1 C1 C2 -172.6(3) . . . . ?
Ca1 O3 C21 Ca1 129.3(5) 2_666 . . . ?
Ca1 O3 C21 O4 13.3(5) . . . . ?
Ca1 O3 C21 O4 142.6(4) 2_666 . . . ?
Ca1 O3 C21 C20 -35.0(7) 2_666 . . . ?
Ca1 O3 C21 C20 -164.4(3) . . . . ?
Ca1 O4 C21 O3 -13.6(5) . . . . ?
Ca1 O4 C21 C20 163.9(4) . . . . ?
Ca1 C1 C2 N1 -169.5(4) . . . . ?
O1 C1 C2 N1 -159.6(4) . . . . ?
O2 C1 C2 N1 22.5(6) . . . . ?
N1 C3 C4 N2 -1.2(5) . . . . ?
N2 C6 C7 C8 112.1(4) . . . . ?
N2 C6 C7 C12 -69.6(5) . . . . ?
N3 C20 C21 Ca1 107.1(12) . . . . ?
N3 C20 C21 O3 -170.9(4) . . . . ?
N3 C20 C21 O4 11.3(6) . . . . ?
N4 C18 C19 N3 0.6(6) . . . . ?
C2 N1 C3 C4 176.7(4) . . . . ?
C2 N1 C5 N2 -176.4(4) . . . . ?
C3 N1 C2 C1 -88.7(5) . . . . ?
C3 N1 C5 N2 -0.7(5) . . . . ?
C4 N2 C5 N1 0.0(5) . . . . ?
C4 N2 C6 C7 160.7(4) . . . . ?
C5 N1 C2 C1 86.1(5) . . . . ?
C5 N1 C3 C4 1.2(5) . . . . ?
C5 N2 C4 C3 0.8(5) . . . . ?
C5 N2 C6 C7 -21.1(6) . . . . ?
C6 N2 C4 C3 179.2(4) . . . . ?
C6 N2 C5 N1 -178.5(4) . . . . ?
C6 C7 C8 C9 177.8(4) . . . . ?
C6 C7 C8 C14 -2.5(6) . . . . ?
C6 C7 C12 C11 -178.8(4) . . . . ?
C6 C7 C12 C15 0.8(6) . . . . ?
C7 C8 C9 C10 1.4(6) . . . . ?
C8 C7 C12 C11 -0.4(6) . . . . ?
C8 C7 C12 C15 179.2(4) . . . . ?
C8 C9 C10 C11 -1.3(6) . . . . ?
C8 C9 C10 C13 178.8(4) . . . . ?
C9 C10 C11 C12 0.3(6) . . . . ?
C9 C10 C11 C16 -179.2(4) . . . . ?
C10 C11 C12 C7 0.6(6) . . . . ?
C10 C11 C12 C15 -179.1(4) . . . . ?
C10 C11 C16 N4 -79.7(5) . . . . ?
C12 C7 C8 C9 -0.5(6) . . . . ?
C12 C7 C8 C14 179.2(4) . . . . ?
C12 C11 C16 N4 100.8(5) . . . . ?
C13 C10 C11 C12 -179.8(4) . . . . ?
C13 C10 C11 C16 0.7(6) . . . . ?
C14 C8 C9 C10 -178.3(4) . . . . ?
C16 N4 C17 N3 -179.4(4) . . . . ?
C16 N4 C18 C19 178.8(4) . . . . ?
C16 C11 C12 C7 -180.0(4) . . . . ?
C16 C11 C12 C15 0.4(6) . . . . ?
C17 N3 C19 C18 -1.0(6) . . . . ?
C17 N3 C20 C21 -91.0(5) . . . . ?
C17 N4 C16 C11 -16.9(6) . . . . ?
C17 N4 C18 C19 0.0(6) . . . . ?
C18 N4 C16 C11 164.5(4) . . . . ?
C18 N4 C17 N3 -0.6(5) . . . . ?
C19 N3 C17 N4 1.0(5) . . . . ?
C19 N3 C20 C21 85.4(5) . . . . ?
C20 N3 C17 N4 177.9(4) . . . . ?
C20 N3 C19 C18 -177.9(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_2
_database_code_depnum_ccdc_archive 'CCDC 1024406'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_audit_creation_date             2015-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        2
_chemical_formula_moiety         
'Br O2, 2(Br), Br O1.77, C58 H72.4 Ca2 N8 O16.2, 4(H2 O)'
_chemical_formula_sum            'C58 H80.40 Br4 Ca2 N8 O23.97'
_chemical_formula_weight         1673.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.1675(7)
_cell_length_b                   16.5118(9)
_cell_length_c                   17.3328(8)
_cell_angle_alpha                94.247(4)
_cell_angle_beta                 109.921(4)
_cell_angle_gamma                110.838(5)
_cell_volume                     3473.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13074
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.85
_cell_measurement_theta_min      3.57
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.821
_exptl_absorpt_correction_T_max  0.560
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26432
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.853
_diffrn_reflns_theta_min         3.569
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10119
_reflns_number_total             13074
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         2.649
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         13074
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0652
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1269P)²+6.8602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1920
_refine_ls_wR_factor_ref         0.2107
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H7D-H3AA
 2.2 with sigma of 0.02
 H7C-H3AA
 2.2 with sigma of 0.02
 H3AB-H2AB
 2.2 with sigma of 0.02
 H17A-H29A
 2.3 with sigma of 0.02
 H10A-H27A
 2.3 with sigma of 0.02
 H25A-H2BA
 2.2 with sigma of 0.02
 H7D-H4BA
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O3A(0.7) H3AA(0.7) H3AB(0.7) O4A(0.6) H4AA(0.6) H4AB(0.6)
 O6A(0.85) O7(0.5) H7C(0.5) H7D(0.5) O1(0.77) O6B(0.15) O4B(0.4) H4BA(0.4)
 H4BB(0.4)
4.a Free rotating group:
 C19A(C20A,C21A,O2B), C22A(C23A,C24A,C25A,C26A,C27A,C28A,C29A,Ca2,O1B), O9(H9A,
 H9B), O(HA,HB), O2(H2A,H2B,O3)
4.b Rotating group:
 O1A(H1A,H1AA), O2A(H2AA,H2AB), O3A(H3AA,H3AB), O4A(H4AA,H4AB), O2B(H2BA,H2BB),
  O1B(H1BA,H1BB), O9A(H9AA,H9AB), O14(H14A,H14B), O7(H7C,H7D), O4B(H4BA,H4BB)
4.c Secondary CH2 refined with riding coordinates:
 C2A(H2AC,H2AD), C10A(H10A,H10B), C17A(H17A,H17B), C25A(H25A,H25B), C2B(H2BC,
 H2BD), C10B(H10C,H10D), C17B(H17C,H17D), C25B(H25C,H25D)
4.d Me refined with riding coordinates:
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F)
4.e Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C13A(H13A), C18A(H18A),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C3B(H3B), C5B(H5B), C6B(H6B),
 C7B(H7B), C8B(H8B), C13B(H13B), C18B(H18B), C20B(H20B), C21B(H21B), C22B(H22B),
  C23B(H23B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.18450(6) -0.25555(5) 0.02712(5) 0.0567(2) Uani 1 1 d . . . . .
Br2 Br 0.06242(4) 0.31118(4) 0.26592(3) 0.03237(15) Uani 1 1 d . . . . .
Br3 Br -0.56500(4) -0.31100(4) 0.23485(3) 0.03330(15) Uani 1 1 d . . . . .
Br4 Br -0.38641(5) 0.24465(5) 0.34046(4) 0.04715(19) Uani 1 1 d . . . . .
Ca1 Ca -0.28427(8) 0.00904(7) 0.13051(6) 0.0299(2) Uani 1 1 d . . . . .
O1A O -0.3865(3) -0.0354(3) -0.0167(2) 0.0463(10) Uani 1 1 d . . . . .
H1A H -0.4182 -0.0976 -0.0228 0.069 Uiso 1 1 d GR . . . .
H1AA H -0.4400 -0.0331 -0.0622 0.069 Uiso 1 1 d GR . . A 1
O2A O -0.1717(4) -0.0477(4) 0.0712(3) 0.0653(13) Uani 1 1 d . . . . .
H2AA H -0.1662 -0.1038 0.0743 0.098 Uiso 1 1 d GR . . . .
H2AB H -0.1281 -0.0166 0.0421 0.098 Uiso 1 1 d DGR . . . .
O3A O -0.1465(5) 0.1319(4) 0.1052(4) 0.0524(16) Uani 0.7 1 d . . P B .
H3AA H -0.1762 0.1451 0.0555 0.079 Uiso 0.7 1 d DGR . P . .
H3AB H -0.0912 0.1176 0.1041 0.079 Uiso 0.7 1 d DGR . P . .
O4A O -0.2493(7) 0.1502(5) 0.2105(6) 0.0393(18) Uani 0.6 1 d . . P B 1
H4AA H -0.2609 0.1930 0.1881 0.059 Uiso 0.6 1 d GR . P B 1
H4AB H -0.1842 0.1638 0.2483 0.059 Uiso 0.6 1 d GR . P B 1
O5A O -0.3521(3) -0.1502(2) 0.1138(2) 0.0379(8) Uani 1 1 d . . . . .
O8 O -0.4787(3) -0.0273(3) 0.1267(2) 0.0343(8) Uani 1 1 d . . . . .
O7A O -0.1486(3) -0.0021(3) 0.2556(2) 0.0314(8) Uani 1 1 d . . . . .
O6A O -0.4820(6) -0.2083(4) -0.0154(3) 0.0682(19) Uani 0.85 1 d . . P C 1
N1A N -0.5385(3) -0.3756(3) 0.0129(3) 0.0318(9) Uani 1 1 d . . . . .
N2A N -0.7133(3) -0.4632(3) -0.0367(3) 0.0297(9) Uani 1 1 d . . . . .
N3A N -0.8089(3) -0.1727(3) 0.1153(3) 0.0258(8) Uani 1 1 d . . . . .
N4A N -0.6393(3) -0.0801(3) 0.1923(2) 0.0271(8) Uani 1 1 d . . . . .
C1A C -0.4224(5) -0.2143(4) 0.0535(4) 0.0429(13) Uani 1 1 d . . . . .
C2A C -0.4342(4) -0.3041(4) 0.0711(3) 0.0348(11) Uani 1 1 d . . . . .
H2AC H -0.3725 -0.3165 0.0667 0.042 Uiso 1 1 calc R . . . .
H2AD H -0.4294 -0.3037 0.1295 0.042 Uiso 1 1 calc R . . . .
C3A C -0.6317(4) -0.3951(3) 0.0243(3) 0.0316(11) Uani 1 1 d . . . . .
H3A H -0.6392 -0.3650 0.0692 0.038 Uiso 1 1 calc R . . . .
C4A C -0.5582(4) -0.4318(3) -0.0586(3) 0.0309(10) Uani 1 1 d . . . . .
C5A C -0.4894(5) -0.4405(4) -0.0973(4) 0.0387(12) Uani 1 1 d . . . . .
H5A H -0.4137 -0.4021 -0.0764 0.046 Uiso 1 1 calc R . . . .
C6A C -0.5391(6) -0.5088(4) -0.1681(4) 0.0460(15) Uani 1 1 d . . . . .
H6A H -0.4951 -0.5178 -0.1960 0.055 Uiso 1 1 calc R . . . .
C7A C -0.6519(6) -0.5659(4) -0.2011(4) 0.0449(14) Uani 1 1 d . . . . .
H7A H -0.6815 -0.6112 -0.2503 0.054 Uiso 1 1 calc R . . . .
C8A C -0.7194(5) -0.5570(3) -0.1630(3) 0.0365(11) Uani 1 1 d . . . . .
H8A H -0.7954 -0.5949 -0.1846 0.044 Uiso 1 1 calc R . . . .
C9A C -0.6701(4) -0.4890(3) -0.0907(3) 0.0302(10) Uani 1 1 d . . . . .
C10A C -0.8296(4) -0.5033(3) -0.0464(3) 0.0339(11) Uani 1 1 d . . . . .
H10A H -0.8505 -0.5668 -0.0443 0.041 Uiso 1 1 calc DR . . . .
H10B H -0.8773 -0.5000 -0.1020 0.041 Uiso 1 1 calc R . . . .
C11A C -0.8477(4) -0.4562(3) 0.0221(3) 0.0264(10) Uani 1 1 d . . . . .
C12A C -0.8474(4) -0.4898(3) 0.0942(3) 0.0300(10) Uani 1 1 d . . . . .
C13A C -0.8702(4) -0.4484(3) 0.1535(3) 0.0328(11) Uani 1 1 d . . . . .
H13A H -0.8724 -0.4729 0.2011 0.039 Uiso 1 1 calc R . . . .
C14A C -0.8899(4) -0.3726(3) 0.1459(3) 0.0307(10) Uani 1 1 d . . . . .
C15A C -0.8867(4) -0.3371(3) 0.0753(3) 0.0272(10) Uani 1 1 d . . . . .
C16A C -0.8647(4) -0.3781(3) 0.0132(3) 0.0267(10) Uani 1 1 d . . . . .
C17A C -0.9091(4) -0.2541(3) 0.0684(4) 0.0362(12) Uani 1 1 d . . . . .
H17A H -0.9383 -0.2517 0.0084 0.043 Uiso 1 1 calc DR . . . .
H17B H -0.9656 -0.2571 0.0907 0.043 Uiso 1 1 calc R . . . .
C18A C -0.7068(4) -0.1654(3) 0.1590(3) 0.0280(10) Uani 1 1 d . . . . .
H18A H -0.6857 -0.2138 0.1653 0.034 Uiso 1 1 calc R . . . .
C19A C -0.8063(2) -0.08722(18) 0.12159(17) 0.0253(9) Uani 1 1 d . . . . .
C20A C -0.8911(2) -0.0589(2) 0.08898(18) 0.0271(10) Uani 1 1 d G . . . .
H20A H -0.9651 -0.0994 0.0573 0.032 Uiso 1 1 calc R . . . .
C21A C -0.8598(3) 0.0320(2) 0.1060(2) 0.0304(10) Uani 1 1 d G . . . .
H21A H -0.9142 0.0549 0.0857 0.036 Uiso 1 1 calc R . . . .
O2B O -0.3532(2) -0.0633(3) 0.4242(2) 0.0584(13) Uani 1 1 d G . . . .
H2BA H -0.4223 -0.1257 0.3938 0.088 Uiso 1 1 d DGR . . . .
H2BB H -0.3947 -0.0205 0.4224 0.088 Uiso 1 1 d GR . . . .
C22A C -0.75149(13) 0.09093(14) 0.15162(15) 0.0325(11) Uani 1 1 d . . . . .
H22A H -0.7338 0.1529 0.1607 0.039 Uiso 1 1 calc R . . . .
C23A C -0.66773(11) 0.06198(12) 0.18466(13) 0.0304(10) Uani 1 1 d G . . . .
H23A H -0.5937 0.1023 0.2166 0.036 Uiso 1 1 calc R . . . .
C24A C -0.69926(9) -0.02913(11) 0.16794(11) 0.0237(9) Uani 1 1 d G . . . .
C25A C -0.52387(7) -0.04934(8) 0.24786(7) 0.0303(11) Uani 1 1 d G . . . .
H25A H -0.5144 -0.0955 0.2793 0.036 Uiso 1 1 calc DR . . . .
H25B H -0.5034 0.0048 0.2894 0.036 Uiso 1 1 calc R . . . .
C26A C -0.44552(8) -0.02853(8) 0.20294(6) 0.0250(9) Uani 1 1 d G . . . .
C27A C -0.82008(16) -0.56990(8) 0.1099(2) 0.0421(13) Uani 1 1 d G . . . .
H27A H -0.8059 -0.5919 0.0627 0.063 Uiso 1 1 calc DR . . . .
H27B H -0.7546 -0.5524 0.1620 0.063 Uiso 1 1 calc R . . . .
H27C H -0.8821 -0.6169 0.1150 0.063 Uiso 1 1 calc R . . . .
C28A C -0.91112(8) -0.33039(15) 0.21494(16) 0.0494(15) Uani 1 1 d G . . . .
H28A H -0.9236 -0.2776 0.2011 0.074 Uiso 1 1 calc R . . . .
H28B H -0.9761 -0.3731 0.2203 0.074 Uiso 1 1 calc R . . . .
H28C H -0.8473 -0.3131 0.2683 0.074 Uiso 1 1 calc R . . . .
C29A C -0.85849(13) -0.33823(15) -0.06163(12) 0.0412(13) Uani 1 1 d G . . . .
H29A H -0.8724 -0.2843 -0.0578 0.062 Uiso 1 1 calc DR . . . .
H29B H -0.7852 -0.3232 -0.0619 0.062 Uiso 1 1 calc R . . . .
H29C H -0.9138 -0.3813 -0.1137 0.062 Uiso 1 1 calc R . . . .
Ca2 Ca -0.21205(6) -0.02404(6) 0.37100(5) 0.0238(2) Uani 1 1 d G . . . .
O1B O -0.12832(8) 0.03785(9) 0.51999(5) 0.0347(8) Uani 1 1 d G . . . .
H1BA H -0.0738 0.0344 0.5479 0.052 Uiso 1 1 d GR . . . .
H1BB H -0.1023 0.0992 0.5321 0.052 Uiso 1 1 d GR . . . .
O9A O -0.3051(3) -0.1718(3) 0.2775(2) 0.0429(9) Uani 1 1 d . . . . .
H9AA H -0.3566 -0.2281 0.2762 0.064 Uiso 1 1 d GR . . . .
H9AB H -0.3224 -0.1634 0.2256 0.064 Uiso 1 1 d GR . . . .
O5B O -0.1660(3) 0.1364(2) 0.3858(2) 0.0359(8) Uani 1 1 d . . . . .
O6 O -0.0089(3) 0.0336(2) 0.3778(2) 0.0289(7) Uani 1 1 d . . . . .
O7B O -0.3486(3) -0.0129(3) 0.2481(2) 0.0325(8) Uani 1 1 d . . . . .
O8B O -0.0948(3) 0.2074(3) 0.5200(2) 0.0407(9) Uani 1 1 d . . . D 1
N1B N 0.0203(3) 0.3608(3) 0.4793(3) 0.0294(9) Uani 1 1 d . . . . .
N2B N 0.1964(3) 0.4485(3) 0.5411(3) 0.0283(8) Uani 1 1 d . . . . .
N3B N 0.3128(3) 0.1827(3) 0.3785(2) 0.0236(8) Uani 1 1 d . . . . .
N4B N 0.1424(3) 0.0896(3) 0.3038(2) 0.0244(8) Uani 1 1 d . . . . .
C1B C -0.1156(4) 0.2039(3) 0.4427(3) 0.0320(11) Uani 1 1 d . . . . .
C2B C -0.0819(4) 0.2917(3) 0.4155(3) 0.0330(11) Uani 1 1 d . . . . .
H2BC H -0.0718 0.2821 0.3624 0.040 Uiso 1 1 calc R . . . .
H2BD H -0.1416 0.3126 0.4045 0.040 Uiso 1 1 calc R . . . .
C3B C 0.1185(4) 0.3817(3) 0.4760(3) 0.0289(10) Uani 1 1 d . . . . .
H3B H 0.1317 0.3534 0.4335 0.035 Uiso 1 1 calc R . . . .
C4B C 0.0323(4) 0.4162(3) 0.5487(3) 0.0283(10) Uani 1 1 d . . . . .
C5B C -0.0433(5) 0.4245(4) 0.5805(4) 0.0377(12) Uani 1 1 d . . . . .
H5B H -0.1192 0.3862 0.5551 0.045 Uiso 1 1 calc R . . . .
C6B C -0.0011(5) 0.4912(4) 0.6507(4) 0.0418(13) Uani 1 1 d . . . . .
H6B H -0.0503 0.5002 0.6728 0.050 Uiso 1 1 calc R . . . .
C7B C 0.1110(5) 0.5467(4) 0.6913(4) 0.0404(13) Uani 1 1 d . . . . .
H7B H 0.1356 0.5908 0.7404 0.049 Uiso 1 1 calc R . . . .
C8B C 0.1869(4) 0.5384(3) 0.6609(3) 0.0327(11) Uani 1 1 d . . . . .
H8B H 0.2631 0.5755 0.6878 0.039 Uiso 1 1 calc R . . . .
C9B C 0.1444(4) 0.4724(3) 0.5887(3) 0.0280(10) Uani 1 1 d . . . . .
C10B C 0.3152(4) 0.4903(3) 0.5584(3) 0.0328(11) Uani 1 1 d . . . . .
H10C H 0.3573 0.4786 0.6117 0.039 Uiso 1 1 calc R . . . .
H10D H 0.3388 0.5555 0.5656 0.039 Uiso 1 1 calc R . . . .
C11B C 0.3408(4) 0.4556(3) 0.4884(3) 0.0261(9) Uani 1 1 d . . . . .
C12B C 0.3430(4) 0.4993(3) 0.4227(3) 0.0282(10) Uani 1 1 d . . . . .
C13B C 0.3649(4) 0.4656(3) 0.3578(3) 0.0296(10) Uani 1 1 d . . . . .
H13B H 0.3661 0.4957 0.3133 0.035 Uiso 1 1 calc R . . . .
C14B C 0.3847(4) 0.3899(3) 0.3565(3) 0.0266(9) Uani 1 1 d . . . . .
C15B C 0.3850(4) 0.3459(3) 0.4238(3) 0.0243(9) Uani 1 1 d . . . . .
C16B C 0.3603(4) 0.3777(3) 0.4885(3) 0.0251(9) Uani 1 1 d . . . . .
C17B C 0.4115(4) 0.2651(3) 0.4240(3) 0.0284(10) Uani 1 1 d . . . . .
H17C H 0.4649 0.2718 0.3974 0.034 Uiso 1 1 calc R . . . .
H17D H 0.4464 0.2610 0.4829 0.034 Uiso 1 1 calc R . . . .
C18B C 0.2107(4) 0.1750(3) 0.3366(3) 0.0252(9) Uani 1 1 d . . . . .
H18B H 0.1895 0.2235 0.3308 0.030 Uiso 1 1 calc R . . . .
C19B C 0.3111(4) 0.0977(3) 0.3735(3) 0.0215(9) Uani 1 1 d . . . . .
C20B C 0.3953(4) 0.0688(3) 0.4046(3) 0.0262(9) Uani 1 1 d . . . . .
H20B H 0.4698 0.1094 0.4346 0.031 Uiso 1 1 calc R . . . .
C21B C 0.3643(4) -0.0221(3) 0.3895(3) 0.0290(10) Uani 1 1 d . . . . .
H21B H 0.4185 -0.0450 0.4107 0.035 Uiso 1 1 calc R . . . .
C22B C 0.2553(4) -0.0810(3) 0.3438(3) 0.0316(11) Uani 1 1 d . . . . .
H22B H 0.2379 -0.1430 0.3351 0.038 Uiso 1 1 calc R . . . .
C23B C 0.1713(4) -0.0535(3) 0.3107(3) 0.0284(10) Uani 1 1 d . . . . .
H23B H 0.0972 -0.0942 0.2794 0.034 Uiso 1 1 calc R . . . .
C24B C 0.2029(4) 0.0383(3) 0.3266(3) 0.0231(9) Uani 1 1 d . . . . .
C25B C 0.0257(4) 0.0580(3) 0.2521(3) 0.0282(10) Uani 1 1 d . . . . .
H25C H 0.0051 0.0075 0.2063 0.034 Uiso 1 1 calc R . . . .
H25D H 0.0122 0.1061 0.2258 0.034 Uiso 1 1 calc R . . . .
C26B C -0.0476(3) 0.0282(3) 0.2999(3) 0.0217(9) Uani 1 1 d . . . . .
C27B C 0.3552(4) 0.3280(4) 0.5583(3) 0.0347(11) Uani 1 1 d . . . . .
H27D H 0.3372 0.3587 0.5982 0.052 Uiso 1 1 calc R . . . .
H27E H 0.2986 0.2674 0.5340 0.052 Uiso 1 1 calc R . . . .
H27F H 0.4266 0.3260 0.5877 0.052 Uiso 1 1 calc R . . . .
C28B C 0.3991(5) 0.3527(4) 0.2811(3) 0.0351(11) Uani 1 1 d . . . . .
H28D H 0.4126 0.2991 0.2895 0.053 Uiso 1 1 calc R . . . .
H28E H 0.3324 0.3376 0.2305 0.053 Uiso 1 1 calc R . . . .
H28F H 0.4618 0.3971 0.2743 0.053 Uiso 1 1 calc R . . . .
C29B C 0.3184(4) 0.5819(3) 0.4180(4) 0.0398(13) Uani 1 1 d . . . . .
H29D H 0.3047 0.5979 0.4675 0.060 Uiso 1 1 calc R . . . .
H29E H 0.3814 0.6312 0.4166 0.060 Uiso 1 1 calc R . . . .
H29F H 0.2533 0.5696 0.3669 0.060 Uiso 1 1 calc R . . . .
O9 O 0.0633(5) 0.1966(3) 0.1079(3) 0.0539(12) Uani 1 1 d . . . . .
H9A H 0.0718 0.2386 0.1463 0.081 Uiso 1 1 d G . . . .
H9B H 0.1151 0.2161 0.0892 0.081 Uiso 1 1 d G . . . .
O14 O -0.1470(3) -0.1269(3) 0.4455(2) 0.0392(9) Uani 1 1 d . . . . .
H14A H -0.0861 -0.0978 0.4970 0.059 Uiso 1 1 d GR . . . .
H14B H -0.1244 -0.1591 0.4138 0.059 Uiso 1 1 d GR . . . .
O O -0.5541(4) -0.1921(3) 0.3964(3) 0.0462(10) Uani 1 1 d . . . . .
HA H -0.5649 -0.2325 0.3553 0.069 Uiso 1 1 d G . . . .
HB H -0.6148 -0.2039 0.4040 0.069 Uiso 1 1 d G . . . .
O0B O -0.2901(4) 0.2246(4) 0.5340(4) 0.0625(14) Uani 1 1 d . . . . .
O2 O -0.1232(4) -0.2672(3) 0.3631(3) 0.0586(12) Uani 1 1 d . . . . .
H2A H -0.1404 -0.2553 0.3133 0.088 Uiso 1 1 d G . . . .
H2B H -0.0526 -0.2399 0.3913 0.088 Uiso 1 1 d G . . . .
O3 O -0.3379(4) 0.2762(3) 0.1657(4) 0.0625(13) Uani 1 1 d G . . . .
O5 O -0.1131(3) -0.2291(3) 0.1622(3) 0.0512(11) Uani 1 1 d . . . . .
O7 O -0.3433(10) 0.1263(9) 0.0552(9) 0.094(4) Uani 0.5 1 d . . P B .
H7C H -0.3504 0.1217 -0.0056 0.140 Uiso 0.5 1 d DGR . P . .
H7D H -0.2918 0.1910 0.0822 0.140 Uiso 0.5 1 d DGR . P . .
O0A O -0.1137(4) -0.1843(4) 0.2296(4) 0.0699(14) Uani 1 1 d . . . . .
O1 O -0.3165(6) 0.2408(9) 0.4775(6) 0.133(5) Uani 0.77 1 d . . P E 1
O6B O -0.410(3) -0.211(3) -0.024(2) 0.070(11) Uani 0.15 1 d . . P C -1
O4B O -0.1917(12) 0.1556(12) 0.2213(8) 0.058(4) Uani 0.4 1 d . . P B -1
H4BA H -0.1719 0.2074 0.2087 0.086 Uiso 0.4 1 d DGR . P B -1
H4BB H -0.1492 0.1410 0.2489 0.086 Uiso 0.4 1 d GR . P B -1
H3C H -0.402(5) 0.254(4) 0.126(4) 0.026(14) Uiso 1 1 d . . . . .
H3D H -0.370(8) 0.246(7) 0.195(7) 0.10(4) Uiso 1 1 d . . . . .


_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
Br1 O5 2.148(4) . ?
Br4 O1 2.256(11) . ?
Ca1 O1A 2.365(4) . ?
Ca1 H1A 2.6940 . ?
Ca1 O2A 2.553(5) . ?
Ca1 O3A 2.453(6) . ?
Ca1 O4A 2.415(8) . ?
Ca1 H4AB 2.7179 . ?
Ca1 O5A 2.413(4) . ?
Ca1 O8 2.579(4) . ?
Ca1 O7A 2.428(3) . ?
Ca1 C26A 2.8707(15) . ?
Ca1 Ca2 4.0679(13) . ?
Ca1 O7B 2.502(3) . ?
Ca1 O7 2.633(12) . ?
Ca1 O4B 2.414(16) . ?
Ca1 H4BB 2.5130 . ?
O1A H1A 0.9448 . ?
O1A H1AA 0.9027 . ?
O2A H2AA 0.9613 . ?
O2A H2AB 0.9613 . ?
O3A H3AA 0.9015 . ?
O3A H3AB 0.9009 . ?
O4A H4AA 0.8699 . ?
O4A H4AB 0.8666 . ?
O4A O4B 0.742(14) . ?
O5A C1A 1.257(7) . ?
O8 C26A 1.247(3) . ?
O7A Ca2 2.459(3) . ?
O7A C26B 1.254(5) . ?
O6A C1A 1.242(8) . ?
O6A O6B 1.09(3) . ?
N1A C2A 1.470(7) . ?
N1A C3A 1.330(6) . ?
N1A C4A 1.374(7) . ?
N2A C3A 1.335(7) . ?
N2A C9A 1.397(6) . ?
N2A C10A 1.482(6) . ?
N3A C17A 1.476(6) . ?
N3A C18A 1.340(6) . ?
N3A C19A 1.394(5) . ?
N4A C18A 1.332(6) . ?
N4A C24A 1.388(4) . ?
N4A C25A 1.457(4) . ?
C1A C2A 1.498(8) . ?
C1A O6B 1.41(4) . ?
C2A H2AC 0.9900 . ?
C2A H2AD 0.9900 . ?
C3A H3A 0.9500 . ?
C4A C5A 1.396(7) . ?
C4A C9A 1.404(7) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.385(8) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.412(9) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.375(8) . ?
C8A H8A 0.9500 . ?
C8A C9A 1.398(7) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10A C11A 1.514(7) . ?
C11A C12A 1.404(7) . ?
C11A C16A 1.404(7) . ?
C12A C13A 1.380(8) . ?
C12A C27A 1.523(5) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.383(7) . ?
C14A C15A 1.402(7) . ?
C14A C28A 1.510(6) . ?
C15A C16A 1.409(7) . ?
C15A C17A 1.517(6) . ?
C16A C29A 1.512(5) . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A H18A 0.9500 . ?
C19A C20A 1.3996 . ?
C19A C24A 1.373(3) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.3813 . ?
C21A H21A 0.9500 . ?
C21A C22A 1.387(4) . ?
O2B H2BA 1.0714 . ?
O2B H2BB 1.0644 . ?
O2B Ca2 2.386(4) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.3949 . ?
C23A H23A 0.9500 . ?
C23A C24A 1.3841 . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C25A C26A 1.5211 . ?
C26A O7B 1.244(3) . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
Ca2 O1B 2.4041 . ?
Ca2 O9A 2.446(4) . ?
Ca2 O5B 2.462(4) . ?
Ca2 O6 2.647(3) . ?
Ca2 O7B 2.412(3) . ?
Ca2 C26B 2.894(4) . ?
Ca2 O14 2.454(4) . ?
O1B H1BA 0.7833 . ?
O1B H1BB 0.9255 . ?
O9A H9AA 0.9491 . ?
O9A H9AB 0.8842 . ?
O5B C1B 1.232(6) . ?
O6 C26B 1.254(5) . ?
O8B C1B 1.261(6) . ?
N1B C2B 1.472(7) . ?
N1B C3B 1.331(6) . ?
N1B C4B 1.378(6) . ?
N2B C3B 1.344(6) . ?
N2B C9B 1.398(6) . ?
N2B C10B 1.482(6) . ?
N3B C17B 1.471(6) . ?
N3B C18B 1.333(6) . ?
N3B C19B 1.391(6) . ?
N4B C18B 1.336(6) . ?
N4B C24B 1.395(6) . ?
N4B C25B 1.455(6) . ?
C1B C2B 1.521(7) . ?
C2B H2BC 0.9900 . ?
C2B H2BD 0.9900 . ?
C3B H3B 0.9500 . ?
C4B C5B 1.403(7) . ?
C4B C9B 1.403(7) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.374(8) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.402(9) . ?
C7B H7B 0.9500 . ?
C7B C8B 1.390(8) . ?
C8B H8B 0.9500 . ?
C8B C9B 1.390(7) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C10B C11B 1.510(7) . ?
C11B C12B 1.395(7) . ?
C11B C16B 1.408(6) . ?
C12B C13B 1.392(7) . ?
C12B C29B 1.524(7) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.377(7) . ?
C14B C15B 1.418(7) . ?
C14B C28B 1.510(7) . ?
C15B C16B 1.403(7) . ?
C15B C17B 1.510(6) . ?
C16B C27B 1.518(7) . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B H18B 0.9500 . ?
C19B C20B 1.395(6) . ?
C19B C24B 1.391(6) . ?
C20B H20B 0.9500 . ?
C20B C21B 1.383(7) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.393(7) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.383(7) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.394(6) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C25B C26B 1.513(6) . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
O9 H9A 0.8689 . ?
O9 H9B 0.8709 . ?
O14 H14A 0.9429 . ?
O14 H14B 0.9412 . ?
O HA 0.8703 . ?
O HB 0.8703 . ?
O0B O1 1.016(12) . ?
O2 H2A 0.8704 . ?
O2 H2B 0.8699 . ?
O3 H3C 0.85(6) . ?
O3 H3D 0.86(10) . ?
O5 O0A 1.340(7) . ?
O7 H7C 1.0193 . ?
O7 H7D 1.0151 . ?
O4B H4BA 0.8693 . ?
O4B H4BB 0.7571 . ?

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
O1A Ca1 H1A 20.2 . . ?
O1A Ca1 O2A 74.84(16) . . ?
O1A Ca1 O3A 88.1(2) . . ?
O1A Ca1 O4A 121.7(2) . . ?
O1A Ca1 H4AB 135.9 . . ?
O1A Ca1 O5A 80.27(14) . . ?
O1A Ca1 O8 80.31(13) . . ?
O1A Ca1 O7A 149.50(14) . . ?
O1A Ca1 C26A 105.10(11) . . ?
O1A Ca1 Ca2 154.17(12) . . ?
O1A Ca1 O7B 129.73(14) . . ?
O1A Ca1 O7 63.0(4) . . ?
O1A Ca1 O4B 129.6(4) . . ?
O1A Ca1 H4BB 143.6 . . ?
H1A Ca1 H4AB 154.9 . . ?
H1A Ca1 H4BB 163.6 . . ?
O2A Ca1 H1A 71.5 . . ?
O2A Ca1 H4AB 120.2 . . ?
O2A Ca1 O8 143.95(15) . . ?
O2A Ca1 C26A 147.85(13) . . ?
O2A Ca1 Ca2 107.66(12) . . ?
O2A Ca1 O7 113.8(3) . . ?
O2A Ca1 H4BB 106.6 . . ?
O3A Ca1 H1A 104.9 . . ?
O3A Ca1 O2A 69.35(18) . . ?
O3A Ca1 H4AB 64.3 . . ?
O3A Ca1 O8 135.84(17) . . ?
O3A Ca1 C26A 142.33(15) . . ?
O3A Ca1 Ca2 117.20(17) . . ?
O3A Ca1 O7B 134.60(19) . . ?
O3A Ca1 O7 61.0(3) . . ?
O3A Ca1 H4BB 60.4 . . ?
O4A Ca1 H1A 138.3 . . ?
O4A Ca1 O2A 134.0(2) . . ?
O4A Ca1 O3A 68.9(2) . . ?
O4A Ca1 H4AB 18.2 . . ?
O4A Ca1 O8 81.5(2) . . ?
O4A Ca1 O7A 86.7(2) . . ?
O4A Ca1 C26A 74.26(19) . . ?
O4A Ca1 Ca2 75.8(2) . . ?
O4A Ca1 O7B 69.4(2) . . ?
O4A Ca1 O7 58.9(4) . . ?
O4A Ca1 H4BB 33.3 . . ?
H4AB Ca1 H4BB 15.2 . . ?
O5A Ca1 H1A 60.1 . . ?
O5A Ca1 O2A 71.03(15) . . ?
O5A Ca1 O3A 140.35(18) . . ?
O5A Ca1 O4A 147.7(2) . . ?
O5A Ca1 H4AB 142.7 . . ?
O5A Ca1 O8 79.44(13) . . ?
O5A Ca1 O7A 79.58(13) . . ?
O5A Ca1 C26A 77.25(10) . . ?
O5A Ca1 Ca2 76.57(9) . . ?
O5A Ca1 O7B 78.28(13) . . ?
O5A Ca1 O7 138.4(3) . . ?
O5A Ca1 O4B 149.6(4) . . ?
O5A Ca1 H4BB 135.5 . . ?
O8 Ca1 H1A 76.2 . . ?
O8 Ca1 H4AB 95.9 . . ?
O8 Ca1 C26A 25.74(8) . . ?
O8 Ca1 Ca2 84.34(8) . . ?
O8 Ca1 O7 75.9(3) . . ?
O8 Ca1 H4BB 108.9 . . ?
O7A Ca1 H1A 134.8 . . ?
O7A Ca1 O2A 77.08(14) . . ?
O7A Ca1 O3A 93.04(18) . . ?
O7A Ca1 H4AB 70.0 . . ?
O7A Ca1 O8 117.85(11) . . ?
O7A Ca1 C26A 92.47(8) . . ?
O7A Ca1 Ca2 33.89(8) . . ?
O7A Ca1 O7B 67.31(11) . . ?
O7A Ca1 O7 141.8(3) . . ?
O7A Ca1 H4BB 57.5 . . ?
C26A Ca1 H1A 97.2 . . ?
C26A Ca1 H4AB 82.9 . . ?
C26A Ca1 Ca2 58.7 . . ?
C26A Ca1 H4BB 92.3 . . ?
Ca2 Ca1 H1A 134.8 . . ?
Ca2 Ca1 H4AB 66.1 . . ?
Ca2 Ca1 H4BB 61.5 . . ?
O7B Ca1 H1A 118.1 . . ?
O7B Ca1 O2A 136.37(15) . . ?
O7B Ca1 H4AB 70.5 . . ?
O7B Ca1 O8 51.36(11) . . ?
O7B Ca1 C26A 25.62(8) . . ?
O7B Ca1 Ca2 33.42(8) . . ?
O7B Ca1 O7 109.8(3) . . ?
O7B Ca1 H4BB 74.9 . . ?
O7 Ca1 H1A 81.6 . . ?
O7 Ca1 H4AB 73.4 . . ?
O7 Ca1 C26A 93.3(3) . . ?
O7 Ca1 Ca2 132.4(3) . . ?
O7 Ca1 H4BB 84.6 . . ?
O4B Ca1 H1A 149.3 . . ?
O4B Ca1 O2A 117.4(4) . . ?
O4B Ca1 O3A 57.9(4) . . ?
O4B Ca1 O4A 17.7(3) . . ?
O4B Ca1 H4AB 7.2 . . ?
O4B Ca1 O8 98.6(4) . . ?
O4B Ca1 O7A 74.6(4) . . ?
O4B Ca1 C26A 88.0(4) . . ?
O4B Ca1 Ca2 73.1(4) . . ?
O4B Ca1 O7B 77.1(4) . . ?
O4B Ca1 O7 67.9(5) . . ?
O4B Ca1 H4BB 17.5 . . ?
Ca1 O1A H1A 99.9 . . ?
Ca1 O1A H1AA 148.5 . . ?
H1A O1A H1AA 96.4 . . ?
Ca1 O2A H2AA 125.3 . . ?
Ca1 O2A H2AB 125.7 . . ?
H2AA O2A H2AB 109.0 . . ?
Ca1 O3A H3AA 111.1 . . ?
Ca1 O3A H3AB 110.7 . . ?
H3AA O3A H3AB 107.8 . . ?
Ca1 O4A H4AA 124.2 . . ?
Ca1 O4A H4AB 101.1 . . ?
H4AA O4A H4AB 116.3 . . ?
O4B O4A Ca1 81.1(16) . . ?
O4B O4A H4AA 111.1 . . ?
O4B O4A H4AB 30.6 . . ?
C1A O5A Ca1 133.4(4) . . ?
C26A O8 Ca1 90.33(18) . . ?
Ca1 O7A Ca2 112.69(13) . . ?
C26B O7A Ca1 143.4(3) . . ?
C26B O7A Ca2 97.1(3) . . ?
O6B O6A C1A 74(2) . . ?
C3A N1A C2A 122.5(4) . . ?
C3A N1A C4A 109.1(4) . . ?
C4A N1A C2A 128.4(4) . . ?
C3A N2A C9A 107.8(4) . . ?
C3A N2A C10A 126.3(4) . . ?
C9A N2A C10A 125.9(4) . . ?
C18A N3A C17A 128.4(4) . . ?
C18A N3A C19A 107.6(4) . . ?
C19A N3A C17A 124.0(3) . . ?
C18A N4A C24A 108.3(3) . . ?
C18A N4A C25A 124.0(4) . . ?
C24A N4A C25A 127.6(3) . . ?
O5A C1A C2A 114.6(5) . . ?
O5A C1A O6B 115.3(18) . . ?
O6A C1A O5A 125.6(6) . . ?
O6A C1A C2A 119.7(5) . . ?
O6A C1A O6B 47.9(13) . . ?
O6B C1A C2A 108.6(17) . . ?
N1A C2A C1A 112.7(5) . . ?
N1A C2A H2AC 109.0 . . ?
N1A C2A H2AD 109.0 . . ?
C1A C2A H2AC 109.0 . . ?
C1A C2A H2AD 109.0 . . ?
H2AC C2A H2AD 107.8 . . ?
N1A C3A N2A 110.3(4) . . ?
N1A C3A H3A 124.9 . . ?
N2A C3A H3A 124.9 . . ?
N1A C4A C5A 132.3(5) . . ?
N1A C4A C9A 106.4(4) . . ?
C5A C4A C9A 121.3(5) . . ?
C4A C5A H5A 122.2 . . ?
C6A C5A C4A 115.6(5) . . ?
C6A C5A H5A 122.2 . . ?
C5A C6A H6A 118.4 . . ?
C5A C6A C7A 123.2(5) . . ?
C7A C6A H6A 118.4 . . ?
C6A C7A H7A 119.4 . . ?
C8A C7A C6A 121.1(5) . . ?
C8A C7A H7A 119.4 . . ?
C7A C8A H8A 121.8 . . ?
C7A C8A C9A 116.3(5) . . ?
C9A C8A H8A 121.8 . . ?
N2A C9A C4A 106.4(4) . . ?
N2A C9A C8A 131.1(5) . . ?
C8A C9A C4A 122.5(5) . . ?
N2A C10A H10A 109.3 . . ?
N2A C10A H10B 109.3 . . ?
N2A C10A C11A 111.5(4) . . ?
H10A C10A H10B 108.0 . . ?
C11A C10A H10A 109.3 . . ?
C11A C10A H10B 109.3 . . ?
C12A C11A C10A 120.7(4) . . ?
C12A C11A C16A 119.8(5) . . ?
C16A C11A C10A 119.5(4) . . ?
C11A C12A C27A 121.6(5) . . ?
C13A C12A C11A 119.6(4) . . ?
C13A C12A C27A 118.8(4) . . ?
C12A C13A H13A 118.9 . . ?
C12A C13A C14A 122.1(5) . . ?
C14A C13A H13A 118.9 . . ?
C13A C14A C15A 118.5(5) . . ?
C13A C14A C28A 118.5(4) . . ?
C15A C14A C28A 123.0(4) . . ?
C14A C15A C16A 120.9(4) . . ?
C14A C15A C17A 117.3(5) . . ?
C16A C15A C17A 121.8(5) . . ?
C11A C16A C15A 119.0(4) . . ?
C11A C16A C29A 120.4(4) . . ?
C15A C16A C29A 120.6(4) . . ?
N3A C17A C15A 111.8(4) . . ?
N3A C17A H17A 109.3 . . ?
N3A C17A H17B 109.3 . . ?
C15A C17A H17A 109.3 . . ?
C15A C17A H17B 109.3 . . ?
H17A C17A H17B 107.9 . . ?
N3A C18A H18A 125.0 . . ?
N4A C18A N3A 110.0(4) . . ?
N4A C18A H18A 125.0 . . ?
N3A C19A C20A 130.2(2) . . ?
C24A C19A N3A 107.2(2) . . ?
C24A C19A C20A 122.63(14) . . ?
C19A C20A H20A 122.3 . . ?
C21A C20A C19A 115.4 . . ?
C21A C20A H20A 122.3 . . ?
C20A C21A H21A 119.0 . . ?
C20A C21A C22A 122.06(14) . . ?
C22A C21A H21A 119.0 . . ?
H2BA O2B H2BB 99.9 . . ?
Ca2 O2B H2BA 117.3 . . ?
Ca2 O2B H2BB 117.5 . . ?
C21A C22A H22A 119.0 . . ?
C21A C22A C23A 122.07(13) . . ?
C23A C22A H22A 119.0 . . ?
C22A C23A H23A 122.1 . . ?
C24A C23A C22A 115.8 . . ?
C24A C23A H23A 122.1 . . ?
C19A C24A N4A 106.9(2) . . ?
C19A C24A C23A 122.00(13) . . ?
C23A C24A N4A 131.09(17) . . ?
N4A C25A H25A 108.7 . . ?
N4A C25A H25B 108.7 . . ?
N4A C25A C26A 114.33(16) . . ?
H25A C25A H25B 107.6 . . ?
C26A C25A H25A 108.7 . . ?
C26A C25A H25B 108.7 . . ?
O8 C26A Ca1 63.93(16) . . ?
O8 C26A C25A 120.84(17) . . ?
C25A C26A Ca1 175.1 . . ?
O7B C26A Ca1 60.38(16) . . ?
O7B C26A O8 124.3(2) . . ?
O7B C26A C25A 114.87(16) . . ?
C12A C27A H27A 109.5 . . ?
C12A C27A H27B 109.5 . . ?
C12A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C14A C28A H28A 109.5 . . ?
C14A C28A H28B 109.5 . . ?
C14A C28A H28C 109.5 . . ?
H28A C28A H28B 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C16A C29A H29A 109.5 . . ?
C16A C29A H29B 109.5 . . ?
C16A C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
O7A Ca2 Ca1 33.42(8) . . ?
O7A Ca2 O5B 81.87(13) . . ?
O7A Ca2 O6 51.11(10) . . ?
O7A Ca2 C26B 25.48(11) . . ?
O2B Ca2 Ca1 119.34(7) . . ?
O2B Ca2 O7A 152.01(10) . . ?
O2B Ca2 O1B 71.83(9) . . ?
O2B Ca2 O9A 89.18(16) . . ?
O2B Ca2 O5B 99.31(16) . . ?
O2B Ca2 O6 156.84(10) . . ?
O2B Ca2 O7B 84.89(10) . . ?
O2B Ca2 C26B 176.75(12) . . ?
O2B Ca2 O14 87.84(13) . . ?
O1B Ca2 Ca1 150.2 . . ?
O1B Ca2 O7A 134.06(8) . . ?
O1B Ca2 O9A 137.38(10) . . ?
O1B Ca2 O5B 74.49(9) . . ?
O1B Ca2 O6 85.75(8) . . ?
O1B Ca2 O7B 137.75(9) . . ?
O1B Ca2 C26B 109.92(9) . . ?
O1B Ca2 O14 70.53(10) . . ?
O9A Ca2 Ca1 72.38(9) . . ?
O9A Ca2 O7A 76.53(13) . . ?
O9A Ca2 O5B 147.64(13) . . ?
O9A Ca2 O6 104.19(13) . . ?
O9A Ca2 C26B 91.15(14) . . ?
O9A Ca2 O14 70.98(13) . . ?
O5B Ca2 Ca1 76.29(9) . . ?
O5B Ca2 O6 79.57(12) . . ?
O5B Ca2 C26B 78.74(13) . . ?
O6 Ca2 Ca1 83.12(7) . . ?
O6 Ca2 C26B 25.67(11) . . ?
O7B Ca2 Ca1 34.83(8) . . ?
O7B Ca2 O7A 68.25(11) . . ?
O7B Ca2 O9A 74.54(13) . . ?
O7B Ca2 O5B 75.20(13) . . ?
O7B Ca2 O6 116.64(11) . . ?
O7B Ca2 C26B 92.08(12) . . ?
O7B Ca2 O14 144.83(14) . . ?
C26B Ca2 Ca1 57.76(9) . . ?
O14 Ca2 Ca1 133.43(10) . . ?
O14 Ca2 O7A 109.34(13) . . ?
O14 Ca2 O5B 139.97(13) . . ?
O14 Ca2 O6 79.05(12) . . ?
O14 Ca2 C26B 95.33(13) . . ?
Ca2 O1B H1BA 120.3 . . ?
Ca2 O1B H1BB 112.1 . . ?
H1BA O1B H1BB 97.4 . . ?
Ca2 O9A H9AA 136.0 . . ?
Ca2 O9A H9AB 106.4 . . ?
H9AA O9A H9AB 108.2 . . ?
C1B O5B Ca2 137.7(3) . . ?
C26B O6 Ca2 88.2(3) . . ?
C26A O7B Ca1 94.00(18) . . ?
C26A O7B Ca2 151.8(2) . . ?
Ca2 O7B Ca1 111.74(13) . . ?
C3B N1B C2B 123.6(4) . . ?
C3B N1B C4B 108.5(4) . . ?
C4B N1B C2B 127.9(4) . . ?
C3B N2B C9B 107.3(4) . . ?
C3B N2B C10B 126.4(4) . . ?
C9B N2B C10B 126.2(4) . . ?
C18B N3B C17B 127.4(4) . . ?
C18B N3B C19B 108.0(4) . . ?
C19B N3B C17B 124.7(4) . . ?
C18B N4B C24B 108.2(4) . . ?
C18B N4B C25B 124.7(4) . . ?
C24B N4B C25B 127.1(4) . . ?
O5B C1B O8B 126.6(5) . . ?
O5B C1B C2B 116.0(5) . . ?
O8B C1B C2B 117.3(5) . . ?
N1B C2B C1B 112.5(4) . . ?
N1B C2B H2BC 109.1 . . ?
N1B C2B H2BD 109.1 . . ?
C1B C2B H2BC 109.1 . . ?
C1B C2B H2BD 109.1 . . ?
H2BC C2B H2BD 107.8 . . ?
N1B C3B N2B 110.7(4) . . ?
N1B C3B H3B 124.6 . . ?
N2B C3B H3B 124.6 . . ?
N1B C4B C5B 132.4(5) . . ?
N1B C4B C9B 106.9(4) . . ?
C9B C4B C5B 120.7(5) . . ?
C4B C5B H5B 122.0 . . ?
C6B C5B C4B 116.0(5) . . ?
C6B C5B H5B 122.0 . . ?
C5B C6B H6B 118.4 . . ?
C5B C6B C7B 123.3(5) . . ?
C7B C6B H6B 118.4 . . ?
C6B C7B H7B 119.4 . . ?
C8B C7B C6B 121.2(5) . . ?
C8B C7B H7B 119.4 . . ?
C7B C8B H8B 122.1 . . ?
C7B C8B C9B 115.8(5) . . ?
C9B C8B H8B 122.1 . . ?
N2B C9B C4B 106.6(4) . . ?
C8B C9B N2B 130.4(5) . . ?
C8B C9B C4B 123.0(5) . . ?
N2B C10B H10C 109.2 . . ?
N2B C10B H10D 109.2 . . ?
N2B C10B C11B 112.0(4) . . ?
H10C C10B H10D 107.9 . . ?
C11B C10B H10C 109.2 . . ?
C11B C10B H10D 109.2 . . ?
C12B C11B C10B 120.3(4) . . ?
C12B C11B C16B 119.9(4) . . ?
C16B C11B C10B 119.7(4) . . ?
C11B C12B C29B 121.9(5) . . ?
C13B C12B C11B 119.7(4) . . ?
C13B C12B C29B 118.4(5) . . ?
C12B C13B H13B 119.2 . . ?
C14B C13B C12B 121.7(5) . . ?
C14B C13B H13B 119.2 . . ?
C13B C14B C15B 119.2(5) . . ?
C13B C14B C28B 119.1(4) . . ?
C15B C14B C28B 121.6(4) . . ?
C14B C15B C17B 119.0(4) . . ?
C16B C15B C14B 119.8(4) . . ?
C16B C15B C17B 121.2(4) . . ?
C11B C16B C27B 120.6(4) . . ?
C15B C16B C11B 119.7(4) . . ?
C15B C16B C27B 119.7(4) . . ?
N3B C17B C15B 111.9(4) . . ?
N3B C17B H17C 109.2 . . ?
N3B C17B H17D 109.2 . . ?
C15B C17B H17C 109.2 . . ?
C15B C17B H17D 109.2 . . ?
H17C C17B H17D 107.9 . . ?
N3B C18B N4B 110.4(4) . . ?
N3B C18B H18B 124.8 . . ?
N4B C18B H18B 124.8 . . ?
N3B C19B C20B 131.1(4) . . ?
C24B C19B N3B 107.1(4) . . ?
C24B C19B C20B 121.7(4) . . ?
C19B C20B H20B 121.9 . . ?
C21B C20B C19B 116.2(4) . . ?
C21B C20B H20B 121.9 . . ?
C20B C21B H21B 119.2 . . ?
C20B C21B C22B 121.5(4) . . ?
C22B C21B H21B 119.2 . . ?
C21B C22B H22B 118.5 . . ?
C23B C22B C21B 123.0(5) . . ?
C23B C22B H22B 118.5 . . ?
C22B C23B H23B 122.4 . . ?
C22B C23B C24B 115.2(4) . . ?
C24B C23B H23B 122.4 . . ?
C19B C24B N4B 106.3(4) . . ?
C19B C24B C23B 122.3(4) . . ?
C23B C24B N4B 131.4(4) . . ?
N4B C25B H25C 108.7 . . ?
N4B C25B H25D 108.7 . . ?
N4B C25B C26B 114.1(4) . . ?
H25C C25B H25D 107.6 . . ?
C26B C25B H25C 108.7 . . ?
C26B C25B H25D 108.7 . . ?
O7A C26B Ca2 57.5(2) . . ?
O7A C26B C25B 114.7(4) . . ?
O6 C26B O7A 123.4(4) . . ?
O6 C26B Ca2 66.1(2) . . ?
O6 C26B C25B 121.8(4) . . ?
C25B C26B Ca2 171.4(3) . . ?
C16B C27B H27D 109.5 . . ?
C16B C27B H27E 109.5 . . ?
C16B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C14B C28B H28D 109.5 . . ?
C14B C28B H28E 109.5 . . ?
C14B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C12B C29B H29D 109.5 . . ?
C12B C29B H29E 109.5 . . ?
C12B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
H9A O9 H9B 109.4 . . ?
Ca2 O14 H14A 113.0 . . ?
Ca2 O14 H14B 112.2 . . ?
H14A O14 H14B 105.8 . . ?
HA O HB 109.5 . . ?
H2A O2 H2B 109.3 . . ?
H3C O3 H3D 85(7) . . ?
O0A O5 Br1 140.6(4) . . ?
Ca1 O7 H7C 115.5 . . ?
Ca1 O7 H7D 115.6 . . ?
H7C O7 H7D 102.6 . . ?
O0B O1 Br4 167.2(12) . . ?
O6A O6B C1A 57.7(17) . . ?
Ca1 O4B H4BA 129.6 . . ?
Ca1 O4B H4BB 88.7 . . ?
O4A O4B Ca1 81.2(16) . . ?
O4A O4B H4BA 93.5 . . ?
O4A O4B H4BB 141.4 . . ?
H4BA O4B H4BB 120.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O5A C1A O6A -4.8(11) . . . . ?
Ca1 O5A C1A C2A 177.3(3) . . . . ?
Ca1 O5A C1A O6B 50.2(17) . . . . ?
Ca1 O8 C26A C25A -178.89(6) . . . . ?
Ca1 O8 C26A O7B 1.6(3) . . . . ?
Ca1 O7A C26B Ca2 145.0(6) . . . . ?
Ca1 O7A C26B O6 149.5(4) . . . . ?
Ca1 O7A C26B C25B -30.8(7) . . . . ?
Ca1 C26A O7B Ca2 -156.4(6) . . . . ?
O5A C1A C2A N1A 160.8(5) . . . . ?
O5A C1A O6B O6A -116.2(16) . . . . ?
O8 C26A O7B Ca1 -1.7(3) . . . . ?
O8 C26A O7B Ca2 -158.0(5) . . . . ?
O6A C1A C2A N1A -17.2(9) . . . . ?
N1A C4A C5A C6A 177.3(5) . . . . ?
N1A C4A C9A N2A 0.8(5) . . . . ?
N1A C4A C9A C8A -178.7(5) . . . . ?
N2A C10A C11A C12A -96.7(5) . . . . ?
N2A C10A C11A C16A 83.2(5) . . . . ?
N3A C19A C20A C21A -179.0(4) . . . . ?
N3A C19A C24A N4A -2.6(4) . . . . ?
N3A C19A C24A C23A 178.8(2) . . . . ?
N4A C25A C26A O8 9.0(3) . . . . ?
N4A C25A C26A O7B -171.5(3) . . . . ?
C2A N1A C3A N2A -179.1(5) . . . . ?
C2A N1A C4A C5A 1.0(9) . . . . ?
C2A N1A C4A C9A 178.9(5) . . . . ?
C2A C1A O6B O6A 113.6(15) . . . . ?
C3A N1A C2A C1A -82.8(6) . . . . ?
C3A N1A C4A C5A -178.7(6) . . . . ?
C3A N1A C4A C9A -0.8(6) . . . . ?
C3A N2A C9A C4A -0.4(6) . . . . ?
C3A N2A C9A C8A 178.9(5) . . . . ?
C3A N2A C10A C11A 1.0(7) . . . . ?
C4A N1A C2A C1A 97.5(6) . . . . ?
C4A N1A C3A N2A 0.6(6) . . . . ?
C4A C5A C6A C7A 1.0(9) . . . . ?
C5A C4A C9A N2A 178.9(5) . . . . ?
C5A C4A C9A C8A -0.5(8) . . . . ?
C5A C6A C7A C8A -0.8(9) . . . . ?
C6A C7A C8A C9A -0.1(8) . . . . ?
C7A C8A C9A N2A -178.6(5) . . . . ?
C7A C8A C9A C4A 0.7(8) . . . . ?
C9A N2A C3A N1A -0.1(6) . . . . ?
C9A N2A C10A C11A -177.9(4) . . . . ?
C9A C4A C5A C6A -0.4(8) . . . . ?
C10A N2A C3A N1A -179.1(5) . . . . ?
C10A N2A C9A C4A 178.6(5) . . . . ?
C10A N2A C9A C8A -2.0(9) . . . . ?
C10A C11A C12A C13A -176.4(4) . . . . ?
C10A C11A C12A C27A 4.9(6) . . . . ?
C10A C11A C16A C15A 177.0(4) . . . . ?
C10A C11A C16A C29A -3.6(6) . . . . ?
C11A C12A C13A C14A -2.2(7) . . . . ?
C12A C11A C16A C15A -3.0(7) . . . . ?
C12A C11A C16A C29A 176.3(4) . . . . ?
C12A C13A C14A C15A 0.1(7) . . . . ?
C12A C13A C14A C28A -178.4(4) . . . . ?
C13A C14A C15A C16A 0.5(7) . . . . ?
C13A C14A C15A C17A 179.8(4) . . . . ?
C14A C15A C16A C11A 1.0(7) . . . . ?
C14A C15A C16A C29A -178.4(4) . . . . ?
C14A C15A C17A N3A 85.1(6) . . . . ?
C16A C11A C12A C13A 3.7(7) . . . . ?
C16A C11A C12A C27A -175.0(4) . . . . ?
C16A C15A C17A N3A -95.7(6) . . . . ?
C17A N3A C18A N4A -180.0(5) . . . . ?
C17A N3A C19A C20A 1.1(6) . . . . ?
C17A N3A C19A C24A -178.5(4) . . . . ?
C17A C15A C16A C11A -178.3(4) . . . . ?
C17A C15A C16A C29A 2.4(6) . . . . ?
C18A N3A C17A C15A 1.3(8) . . . . ?
C18A N3A C19A C20A -178.6(3) . . . . ?
C18A N3A C19A C24A 1.8(4) . . . . ?
C18A N4A C24A C19A 2.4(4) . . . . ?
C18A N4A C24A C23A -179.1(2) . . . . ?
C18A N4A C25A C26A 92.2(4) . . . . ?
C19A N3A C17A C15A -178.2(4) . . . . ?
C19A N3A C18A N4A -0.4(5) . . . . ?
C19A C20A C21A C22A 0.6(4) . . . . ?
C20A C19A C24A N4A 177.8(2) . . . . ?
C20A C19A C24A C23A -0.9(2) . . . . ?
C20A C21A C22A C23A -1.3(5) . . . . ?
C21A C22A C23A C24A 0.9(3) . . . . ?
C22A C23A C24A N4A -178.2(2) . . . . ?
C22A C23A C24A C19A 0.1(2) . . . . ?
C24A N4A C18A N3A -1.3(5) . . . . ?
C24A N4A C25A C26A -91.1(4) . . . . ?
C24A C19A C20A C21A 0.51(15) . . . . ?
C25A N4A C18A N3A 176.0(3) . . . . ?
C25A N4A C24A C19A -174.7(3) . . . . ?
C25A N4A C24A C23A 3.8(5) . . . . ?
C25A C26A O7B Ca1 178.81(5) . . . . ?
C25A C26A O7B Ca2 22.5(6) . . . . ?
C27A C12A C13A C14A 176.5(4) . . . . ?
C28A C14A C15A C16A 178.9(4) . . . . ?
C28A C14A C15A C17A -1.8(6) . . . . ?
Ca2 O7A C26B O6 4.5(5) . . . . ?
Ca2 O7A C26B C25B -175.8(3) . . . . ?
Ca2 O5B C1B O8B -21.8(9) . . . . ?
Ca2 O5B C1B C2B 162.3(3) . . . . ?
Ca2 O6 C26B O7A -4.1(5) . . . . ?
Ca2 O6 C26B C25B 176.2(4) . . . . ?
O5B C1B C2B N1B -149.5(5) . . . . ?
O8B C1B C2B N1B 34.2(6) . . . . ?
N1B C4B C5B C6B -177.2(5) . . . . ?
N1B C4B C9B N2B 0.1(5) . . . . ?
N1B C4B C9B C8B 179.0(4) . . . . ?
N2B C10B C11B C12B 92.5(5) . . . . ?
N2B C10B C11B C16B -86.3(5) . . . . ?
N3B C19B C20B C21B 178.7(4) . . . . ?
N3B C19B C24B N4B 0.6(5) . . . . ?
N3B C19B C24B C23B -178.6(4) . . . . ?
N4B C25B C26B O7A -177.7(4) . . . . ?
N4B C25B C26B O6 2.1(7) . . . . ?
C2B N1B C3B N2B 178.4(4) . . . . ?
C2B N1B C4B C5B 0.8(9) . . . . ?
C2B N1B C4B C9B -178.1(4) . . . . ?
C3B N1B C2B C1B 98.8(6) . . . . ?
C3B N1B C4B C5B 178.4(5) . . . . ?
C3B N1B C4B C9B -0.5(5) . . . . ?
C3B N2B C9B C4B 0.3(5) . . . . ?
C3B N2B C9B C8B -178.5(5) . . . . ?
C3B N2B C10B C11B 5.7(7) . . . . ?
C4B N1B C2B C1B -84.0(6) . . . . ?
C4B N1B C3B N2B 0.7(6) . . . . ?
C4B C5B C6B C7B -2.3(8) . . . . ?
C5B C4B C9B N2B -178.9(5) . . . . ?
C5B C4B C9B C8B 0.0(8) . . . . ?
C5B C6B C7B C8B 1.6(9) . . . . ?
C6B C7B C8B C9B 0.0(8) . . . . ?
C7B C8B C9B N2B 177.8(5) . . . . ?
C7B C8B C9B C4B -0.8(7) . . . . ?
C9B N2B C3B N1B -0.6(6) . . . . ?
C9B N2B C10B C11B -172.9(4) . . . . ?
C9B C4B C5B C6B 1.5(8) . . . . ?
C10B N2B C3B N1B -179.5(4) . . . . ?
C10B N2B C9B C4B 179.1(4) . . . . ?
C10B N2B C9B C8B 0.3(8) . . . . ?
C10B C11B C12B C13B -178.9(4) . . . . ?
C10B C11B C12B C29B -1.0(7) . . . . ?
C10B C11B C16B C15B -179.5(4) . . . . ?
C10B C11B C16B C27B 0.4(7) . . . . ?
C11B C12B C13B C14B -0.1(7) . . . . ?
C12B C11B C16B C15B 1.7(7) . . . . ?
C12B C11B C16B C27B -178.4(4) . . . . ?
C12B C13B C14B C15B -1.2(7) . . . . ?
C12B C13B C14B C28B 175.3(4) . . . . ?
C13B C14B C15B C16B 2.8(7) . . . . ?
C13B C14B C15B C17B -177.4(4) . . . . ?
C14B C15B C16B C11B -3.1(7) . . . . ?
C14B C15B C16B C27B 177.1(4) . . . . ?
C14B C15B C17B N3B -88.6(5) . . . . ?
C16B C11B C12B C13B -0.1(7) . . . . ?
C16B C11B C12B C29B 177.8(4) . . . . ?
C16B C15B C17B N3B 91.2(5) . . . . ?
C17B N3B C18B N4B -179.6(4) . . . . ?
C17B N3B C19B C20B -2.4(8) . . . . ?
C17B N3B C19B C24B 179.0(4) . . . . ?
C17B C15B C16B C11B 177.2(4) . . . . ?
C17B C15B C16B C27B -2.7(7) . . . . ?
C18B N3B C17B C15B 3.7(7) . . . . ?
C18B N3B C19B C20B 178.5(5) . . . . ?
C18B N3B C19B C24B -0.1(5) . . . . ?
C18B N4B C24B C19B -0.9(5) . . . . ?
C18B N4B C24B C23B 178.2(5) . . . . ?
C18B N4B C25B C26B -97.8(5) . . . . ?
C19B N3B C17B C15B -175.3(4) . . . . ?
C19B N3B C18B N4B -0.5(5) . . . . ?
C19B C20B C21B C22B 1.5(7) . . . . ?
C20B C19B C24B N4B -178.1(4) . . . . ?
C20B C19B C24B C23B 2.7(7) . . . . ?
C20B C21B C22B C23B 0.0(8) . . . . ?
C21B C22B C23B C24B -0.3(7) . . . . ?
C22B C23B C24B N4B -180.0(4) . . . . ?
C22B C23B C24B C19B -1.0(7) . . . . ?
C24B N4B C18B N3B 0.9(5) . . . . ?
C24B N4B C25B C26B 83.5(6) . . . . ?
C24B C19B C20B C21B -2.8(6) . . . . ?
C25B N4B C18B N3B -178.0(4) . . . . ?
C25B N4B C24B C19B 178.0(4) . . . . ?
C25B N4B C24B C23B -2.9(8) . . . . ?
C28B C14B C15B C16B -173.6(4) . . . . ?
C28B C14B C15B C17B 6.2(7) . . . . ?
C29B C12B C13B C14B -178.1(4) . . . . ?
O6B O6A C1A O5A 93(2) . . . . ?
O6B O6A C1A C2A -89(2) . . . . ?
O6B C1A C2A N1A -68.7(17) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_3
_database_code_depnum_ccdc_archive 'CCDC 1024407'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_audit_creation_date             2015-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        3
_chemical_formula_moiety         'Br, 0.5(C36 H44 Ca2 N8 O12)'
_chemical_formula_sum            'C18 H22 Br Ca N4 O6'
_chemical_formula_weight         510.38
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   11.8051(15)
_cell_length_b                   14.1508(16)
_cell_length_c                   7.6915(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.038(9)
_cell_angle_gamma                90
_cell_volume                     1284.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2326
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.67
_cell_measurement_theta_min      3.12
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.242
_exptl_absorpt_correction_T_max  0.4222
_exptl_absorpt_correction_T_min  0.3643
_exptl_absorpt_correction_type   Sphere
_exptl_absorpt_process_details   
;
C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_size_rad          0.1630
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2326
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        68.700
_diffrn_reflns_theta_max         70.666
_diffrn_reflns_theta_min         3.123
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Fine focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1324
_reflns_number_total             2326
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0697
_refine_ls_restrained_S_all      0.952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1269P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2293
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O1A(0.7) H1AA(0.7) H1AB(0.7) O1B(0.3) H1BA(0.3) H1BB(0.3)
3.a Rotating group:
 O1A(H1AA,H1AB), O1B(H1BA,H1BB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.5000 1.11565(7) 0.7500 0.1027(5) Uani 1 2 d S T P . .
Ca1 Ca 0.5000 1.46819(11) 0.7500 0.0940(7) Uani 1 2 d S T P . .
O3 O 0.3766(7) 1.3927(5) 0.2231(6) 0.171(3) Uani 1 1 d . . . . .
O2 O 0.4043(6) 1.4387(5) 0.4884(5) 0.153(2) Uani 1 1 d . . . . .
N1 N 0.2888(6) 1.2243(5) 0.3171(7) 0.113(2) Uani 1 1 d . . . . .
N2 N 0.2430(5) 1.1570(5) 0.0790(6) 0.0993(15) Uani 1 1 d . . . . .
C1 C 0.3663(8) 1.3807(6) 0.3772(8) 0.132(3) Uani 1 1 d . . . . .
C2 C 0.3001(9) 1.2978(6) 0.4475(9) 0.135(3) Uani 1 1 d . . . . .
H2A H 0.3387 1.2727 0.5498 0.162 Uiso 1 1 calc R . . . .
H2B H 0.2254 1.3189 0.4813 0.162 Uiso 1 1 calc R . . . .
C3 C 0.3592(6) 1.1507(8) 0.2996(9) 0.113(2) Uani 1 1 d . . . . .
H3 H 0.4189 1.1360 0.3754 0.135 Uiso 1 1 calc R . . . .
C4 C 0.3309(6) 1.1015(6) 0.1574(9) 0.111(2) Uani 1 1 d . . . . .
H4 H 0.3612 1.0448 0.1187 0.134 Uiso 1 1 calc R . . . .
C5 C 0.2209(6) 1.2275(6) 0.1796(8) 0.105(2) Uani 1 1 d . . . . .
H5 H 0.1658 1.2732 0.1583 0.126 Uiso 1 1 calc R . . . .
C6 C 0.1813(6) 1.1302(5) -0.0797(7) 0.102(2) Uani 1 1 d . . . . .
H6A H 0.2332 1.1009 -0.1598 0.122 Uiso 1 1 calc R . . . .
H6B H 0.1504 1.1864 -0.1350 0.122 Uiso 1 1 calc R . . . .
C7 C 0.0862(5) 1.0623(6) -0.0411(6) 0.0905(17) Uani 1 1 d . . . . .
C8 C -0.0173(7) 1.0979(6) -0.0031(8) 0.106(2) Uani 1 1 d . . . . .
H8 H -0.0302 1.1627 -0.0033 0.127 Uiso 1 1 calc R . . . .
C9 C -0.1068(6) 1.0326(6) 0.0376(8) 0.102(2) Uani 1 1 d . . . . .
H9 H -0.1788 1.0552 0.0616 0.123 Uiso 1 1 calc R . . . .
O1A O 0.4058(11) 1.3329(7) 0.8699(9) 0.147(4) Uani 0.7 1 d . . . A 1
H1AA H 0.3891 1.2820 0.8161 0.220 Uiso 0.7 1 d GR . . A 1
H1AB H 0.4541 1.3192 0.9535 0.220 Uiso 0.7 1 d GR . . A 1
O1B O 0.3237(19) 1.3853(13) 0.8638(17) 0.109(5) Uani 0.3 1 d . . . A -1
H1BA H 0.2411 1.3982 0.8852 0.164 Uiso 0.3 1 d GR . . A -1
H1BB H 0.3476 1.4278 0.9340 0.164 Uiso 0.3 1 d GR . . A -1


_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
Ca1 Ca1 3.9497(7) 3_687 ?
Ca1 O3 2.455(6) 3_686 ?
Ca1 O3 2.455(6) 4_586 ?
Ca1 O2 2.327(5) 2_656 ?
Ca1 O2 2.327(5) . ?
Ca1 O2 2.540(5) 4_586 ?
Ca1 O2 2.540(5) 3_686 ?
Ca1 C1 2.842(8) 3_686 ?
Ca1 C1 2.842(8) 4_586 ?
Ca1 O1A 2.405(8) . ?
Ca1 O1A 2.405(8) 2_656 ?
Ca1 H1AB 2.6867 . ?
Ca1 O1B 2.56(2) . ?
Ca1 H1BB 2.3786 . ?
O3 Ca1 2.455(6) 3_686 ?
O3 C1 1.206(7) . ?
O2 Ca1 2.540(5) 3_686 ?
O2 C1 1.262(8) . ?
N1 C2 1.449(9) . ?
N1 C3 1.340(11) . ?
N1 C5 1.317(9) . ?
N2 C4 1.427(9) . ?
N2 C5 1.291(9) . ?
N2 C6 1.460(8) . ?
C1 Ca1 2.842(8) 3_686 ?
C1 C2 1.515(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.333(11) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.512(9) . ?
C7 C8 1.358(10) . ?
C7 C9 1.365(10) 3_575 ?
C8 H8 0.9300 . ?
C8 C9 1.441(10) . ?
C9 C7 1.365(10) 3_575 ?
C9 H9 0.9300 . ?
O1A H1AA 0.8521 . ?
O1A H1AB 0.8736 . ?
O1A O1B 1.220(19) . ?
O1B H1BA 1.0092 . ?
O1B H1BB 0.8526 . ?

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
Ca1 Ca1 H1AB 66.9 3_687 . ?
Ca1 Ca1 H1BB 57.5 3_687 . ?
O3 Ca1 Ca1 75.28(11) 3_686 3_687 ?
O3 Ca1 Ca1 83.62(11) 4_586 3_687 ?
O3 Ca1 O3 73.5(4) 3_686 4_586 ?
O3 Ca1 O2 78.1(3) 3_686 4_586 ?
O3 Ca1 O2 51.23(15) 4_586 4_586 ?
O3 Ca1 O2 51.23(15) 3_686 3_686 ?
O3 Ca1 O2 78.1(3) 4_586 3_686 ?
O3 Ca1 C1 24.96(16) 4_586 4_586 ?
O3 Ca1 C1 72.6(3) 3_686 4_586 ?
O3 Ca1 C1 72.6(3) 4_586 3_686 ?
O3 Ca1 C1 24.96(16) 3_686 3_686 ?
O3 Ca1 H1AB 134.9 3_686 . ?
O3 Ca1 H1AB 123.5 4_586 . ?
O3 Ca1 O1B 145.5(4) 3_686 . ?
O3 Ca1 O1B 84.9(5) 4_586 . ?
O3 Ca1 H1BB 77.8 4_586 . ?
O3 Ca1 H1BB 126.6 3_686 . ?
O2 Ca1 Ca1 126.34(12) 3_686 3_687 ?
O2 Ca1 Ca1 33.99(12) 4_586 3_687 ?
O2 Ca1 Ca1 150.94(16) . 3_687 ?
O2 Ca1 Ca1 37.60(13) 2_656 3_687 ?
O2 Ca1 O3 78.1(2) 2_656 3_686 ?
O2 Ca1 O3 78.1(2) . 4_586 ?
O2 Ca1 O3 119.65(19) 2_656 4_586 ?
O2 Ca1 O3 119.65(19) . 3_686 ?
O2 Ca1 O2 117.5(3) 4_586 3_686 ?
O2 Ca1 O2 120.1(3) 2_656 3_686 ?
O2 Ca1 O2 120.1(3) . 4_586 ?
O2 Ca1 O2 159.3(4) . 2_656 ?
O2 Ca1 O2 71.6(2) 2_656 4_586 ?
O2 Ca1 O2 71.6(2) . 3_686 ?
O2 Ca1 C1 95.81(19) . 3_686 ?
O2 Ca1 C1 96.6(2) 3_686 4_586 ?
O2 Ca1 C1 95.82(19) 2_656 4_586 ?
O2 Ca1 C1 26.36(15) 4_586 4_586 ?
O2 Ca1 C1 99.7(2) 2_656 3_686 ?
O2 Ca1 C1 99.7(2) . 4_586 ?
O2 Ca1 C1 96.6(3) 4_586 3_686 ?
O2 Ca1 C1 26.36(15) 3_686 3_686 ?
O2 Ca1 O1A 75.3(3) . 2_656 ?
O2 Ca1 O1A 88.2(3) . . ?
O2 Ca1 O1A 88.2(2) 2_656 2_656 ?
O2 Ca1 O1A 75.3(3) 2_656 . ?
O2 Ca1 H1AB 57.0 2_656 . ?
O2 Ca1 H1AB 157.7 3_686 . ?
O2 Ca1 H1AB 83.6 4_586 . ?
O2 Ca1 H1AB 105.2 . . ?
O2 Ca1 O1B 80.1(4) . . ?
O2 Ca1 O1B 90.4(4) 2_656 . ?
O2 Ca1 O1B 149.4(4) 3_686 . ?
O2 Ca1 O1B 67.4(4) 4_586 . ?
O2 Ca1 H1BB 96.4 . . ?
O2 Ca1 H1BB 49.0 4_586 . ?
O2 Ca1 H1BB 154.9 3_686 . ?
O2 Ca1 H1BB 78.6 2_656 . ?
C1 Ca1 Ca1 58.90(13) 4_586 3_687 ?
C1 Ca1 Ca1 99.99(13) 3_686 3_687 ?
C1 Ca1 C1 82.4(4) 3_686 4_586 ?
C1 Ca1 H1AB 105.7 4_586 . ?
C1 Ca1 H1AB 155.5 3_686 . ?
C1 Ca1 H1BB 63.0 4_586 . ?
C1 Ca1 H1BB 144.7 3_686 . ?
O1A Ca1 Ca1 78.46(18) . 3_687 ?
O1A Ca1 Ca1 124.2(2) 2_656 3_687 ?
O1A Ca1 O3 113.1(4) . 4_586 ?
O1A Ca1 O3 152.0(2) . 3_686 ?
O1A Ca1 O3 152.0(2) 2_656 4_586 ?
O1A Ca1 O3 113.1(4) 2_656 3_686 ?
O1A Ca1 O2 85.5(3) . 4_586 ?
O1A Ca1 O2 154.7(2) . 3_686 ?
O1A Ca1 O2 85.5(3) 2_656 3_686 ?
O1A Ca1 O2 154.7(2) 2_656 4_586 ?
O1A Ca1 C1 101.7(4) . 4_586 ?
O1A Ca1 C1 173.7(4) . 3_686 ?
O1A Ca1 C1 101.7(4) 2_656 3_686 ?
O1A Ca1 C1 173.7(4) 2_656 4_586 ?
O1A Ca1 O1A 74.6(6) . 2_656 ?
O1A Ca1 H1AB 18.7 . . ?
O1A Ca1 H1AB 72.5 2_656 . ?
O1A Ca1 O1B 98.7(6) 2_656 . ?
O1A Ca1 O1B 28.3(4) . . ?
O1A Ca1 H1BB 113.4 2_656 . ?
O1A Ca1 H1BB 38.8 . . ?
H1AB Ca1 H1BB 45.7 . . ?
O1B Ca1 Ca1 75.9(3) . 3_687 ?
O1B Ca1 C1 76.5(5) . 4_586 ?
O1B Ca1 C1 157.4(5) . 3_686 ?
O1B Ca1 H1AB 42.8 . . ?
O1B Ca1 H1BB 19.5 . . ?
C1 O3 Ca1 95.8(5) . 3_686 ?
Ca1 O2 Ca1 108.4(2) . 3_686 ?
C1 O2 Ca1 149.7(7) . . ?
C1 O2 Ca1 90.3(4) . 3_686 ?
C3 N1 C2 125.4(7) . . ?
C5 N1 C2 125.3(9) . . ?
C5 N1 C3 108.4(7) . . ?
C4 N2 C6 123.9(6) . . ?
C5 N2 C4 109.0(6) . . ?
C5 N2 C6 126.8(7) . . ?
O3 C1 Ca1 59.3(4) . 3_686 ?
O3 C1 O2 122.2(7) . . ?
O3 C1 C2 121.5(6) . . ?
O2 C1 Ca1 63.3(4) . 3_686 ?
O2 C1 C2 116.2(6) . . ?
C2 C1 Ca1 177.4(7) . 3_686 ?
N1 C2 C1 110.5(6) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 H3 125.0 . . ?
C4 C3 N1 110.0(6) . . ?
C4 C3 H3 125.0 . . ?
N2 C4 H4 128.4 . . ?
C3 C4 N2 103.2(7) . . ?
C3 C4 H4 128.4 . . ?
N1 C5 H5 125.4 . . ?
N2 C5 N1 109.2(8) . . ?
N2 C5 H5 125.4 . . ?
N2 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
N2 C6 C7 111.2(4) . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C8 C7 C6 118.8(7) . . ?
C8 C7 C9 121.4(7) . 3_575 ?
C9 C7 C6 119.8(6) 3_575 . ?
C7 C8 H8 120.8 . . ?
C7 C8 C9 118.3(7) . . ?
C9 C8 H8 120.8 . . ?
C7 C9 C8 120.2(7) 3_575 . ?
C7 C9 H9 119.9 3_575 . ?
C8 C9 H9 119.9 . . ?
Ca1 O1A H1AA 126.2 . . ?
Ca1 O1A H1AB 99.2 . . ?
H1AA O1A H1AB 108.2 . . ?
O1B O1A Ca1 82.8(10) . . ?
O1B O1A H1AA 108.6 . . ?
O1B O1A H1AB 132.1 . . ?
Ca1 O1B H1BA 140.2 . . ?
Ca1 O1B H1BB 68.4 . . ?
O1A O1B Ca1 69.0(11) . . ?
O1A O1B H1BA 150.8 . . ?
O1A O1B H1BB 98.6 . . ?
H1BA O1B H1BB 94.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O3 C1 O2 7.1(12) 3_686 . . . ?
Ca1 O3 C1 C2 -177.0(9) 3_686 . . . ?
Ca1 O2 C1 Ca1 -129.5(12) . . . 3_686 ?
Ca1 O2 C1 O3 -136.2(9) . . . . ?
Ca1 O2 C1 O3 -6.8(11) 3_686 . . . ?
Ca1 O2 C1 C2 177.1(8) 3_686 . . . ?
Ca1 O2 C1 C2 47.6(17) . . . . ?
O3 C1 C2 N1 19.8(14) . . . . ?
O2 C1 C2 N1 -164.1(10) . . . . ?
N1 C3 C4 N2 5.5(8) . . . . ?
N2 C6 C7 C8 89.1(7) . . . . ?
N2 C6 C7 C9 -88.1(7) . . . 3_575 ?
C2 N1 C3 C4 -174.1(7) . . . . ?
C2 N1 C5 N2 171.3(7) . . . . ?
C3 N1 C2 C1 92.9(9) . . . . ?
C3 N1 C5 N2 2.2(8) . . . . ?
C4 N2 C5 N1 1.3(8) . . . . ?
C4 N2 C6 C7 82.7(8) . . . . ?
C5 N1 C2 C1 -74.5(11) . . . . ?
C5 N1 C3 C4 -5.0(8) . . . . ?
C5 N2 C4 C3 -4.2(7) . . . . ?
C5 N2 C6 C7 -89.8(8) . . . . ?
C6 N2 C4 C3 -177.9(6) . . . . ?
C6 N2 C5 N1 174.8(6) . . . . ?
C6 C7 C8 C9 -178.5(5) . . . . ?
C7 C8 C9 C7 1.4(10) . . . 3_575 ?
C9 C7 C8 C9 -1.4(10) 3_575 . . . ?

_smtbx_masks_special_details     
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement. Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 252.5 Ang³ [19.7%]
Total electron count / cell = 111.1
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.410 252.5 111.1 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_4
_database_code_depnum_ccdc_archive 'CCDC 1024408'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        4
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H13 Br0.50 Ca0.50 N2 O3'
_chemical_formula_weight         305.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.6746(12)
_cell_length_b                   11.632(3)
_cell_length_c                   13.537(3)
_cell_angle_alpha                76.891(18)
_cell_angle_beta                 84.108(19)
_cell_angle_gamma                85.173(19)
_cell_volume                     711.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    4503
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      71.07

_exptl_crystal_description       Rectangle
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             313
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    3.930
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_correction_T_min  0.0357
_exptl_absorpt_correction_T_max  0.2366
_exptl_absorpt_process_details   
;
Parkin S,Moezzi B & Hope H, (1995) 
J. Appl. Cryst. 28, 53-56.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'w\ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2562
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.365
_diffrn_reflns_theta_max         71.067
_diffrn_reflns_theta_full        67.700
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             2562
_reflns_number_gt                1964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1223P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2562
_refine_ls_number_parameters     176
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.2054
_refine_ls_wR_factor_gt          0.1897
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.5000 0.5000 0.5000 0.0469(3) Uani 1 2 d S . P . .
Ca1 Ca 0.5000 0.5000 0.0000 0.0592(5) Uani 1 2 d S . P . .
O1 O 0.2002(10) 0.5612(5) 0.1274(3) 0.0707(12) Uani 1 1 d . . . . .
O2 O 0.8381(9) 0.4509(4) 0.1208(3) 0.0607(10) Uani 1 1 d . . . . .
O3 O 0.3391(16) 0.3128(7) 0.0360(4) 0.116(3) Uani 1 1 d . . . . .
H3A H 0.1608 0.2951 0.0488 0.175 Uiso 1 1 d R U . . .
H3B H 0.4486 0.2485 0.0388 0.175 Uiso 1 1 d R U . . .
N4 N 1.1354(9) 0.7856(3) 0.3291(3) 0.0428(9) Uani 1 1 d . . . . .
N6 N 0.8901(10) 0.6838(4) 0.2554(3) 0.0451(9) Uani 1 1 d . . . . .
C1 C 0.9521(13) 0.5278(5) 0.1530(4) 0.0526(13) Uani 1 1 d . . . . .
C2 C 0.7635(13) 0.5833(5) 0.2309(4) 0.0528(13) Uani 1 1 d . . . . .
H2A H 0.5782 0.6099 0.2046 0.063 Uiso 1 1 calc R U . . .
H2B H 0.7303 0.5234 0.2929 0.063 Uiso 1 1 calc R U . . .
C3 C 0.8902(13) 0.7979(5) 0.1957(4) 0.0509(13) Uani 1 1 d . . . . .
H3 H 0.8034 0.8256 0.1353 0.061 Uiso 1 1 calc R U . . .
C4 C 1.0402(13) 0.8604(5) 0.2424(4) 0.0522(13) Uani 1 1 d . . . . .
H4 H 1.0742 0.9401 0.2202 0.063 Uiso 1 1 calc R U . . .
C5 C 1.0421(11) 0.6788(4) 0.3342(3) 0.0410(10) Uani 1 1 d . . . . .
H5 H 1.0778 0.6117 0.3848 0.049 Uiso 1 1 calc R U . . .
C6 C 1.3059(11) 0.8174(4) 0.4045(4) 0.0411(10) Uani 1 1 d . . . . .
H6A H 1.4887 0.8451 0.3709 0.049 Uiso 1 1 calc R U . . .
H6B H 1.3460 0.7475 0.4570 0.049 Uiso 1 1 calc R U . . .
C7 C 1.1505(11) 0.9117(4) 0.4529(3) 0.0378(10) Uani 1 1 d . . . . .
C8 C 0.9413(12) 0.8787(4) 0.5361(4) 0.0422(11) Uani 1 1 d . . . . .
C9 C 0.8707(13) 0.7584(4) 0.5747(4) 0.0481(12) Uani 1 1 d . . . . .
H9 H 0.9630 0.7001 0.5436 0.058 Uiso 1 1 calc R U . . .
C10 C 0.6731(13) 0.7267(4) 0.6552(4) 0.0512(13) Uani 1 1 d . . . . .
H10 H 0.6357 0.6474 0.6792 0.061 Uiso 1 1 calc R U . . .
C11 C 0.5239(13) 0.8130(5) 0.7029(4) 0.0534(13) Uani 1 1 d . . . . .
H11 H 0.3857 0.7909 0.7570 0.064 Uiso 1 1 calc R U . . .
C12 C 0.5831(12) 0.9293(5) 0.6694(4) 0.0486(12) Uani 1 1 d . . . . .
H12 H 0.4876 0.9851 0.7026 0.058 Uiso 1 1 calc R U . . .
C13 C 1.2123(11) 1.0327(4) 0.4152(3) 0.0406(10) Uani 1 1 d . . . . .


_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
Ca1 O3 2.294(6) 2_665 ?
Ca1 O3 2.294(6) . ?
Ca1 O1 2.311(4) . ?
Ca1 O1 2.311(4) 2_665 ?
Ca1 O2 2.335(4) 2_665 ?
Ca1 O2 2.335(4) . ?
Ca1 C1 3.167(6) 2_765 ?
Ca1 C1 3.167(6) 1_455 ?
Ca1 C1 3.190(6) . ?
Ca1 C1 3.190(6) 2_665 ?
O1 C1 1.244(7) 1_455 ?
O2 C1 1.256(7) . ?
O3 H3A 0.8660 . ?
O3 H3B 0.8658 . ?
N4 C5 1.336(6) . ?
N4 C4 1.383(6) . ?
N4 C6 1.484(6) . ?
N6 C5 1.329(6) . ?
N6 C3 1.389(7) . ?
N6 C2 1.469(7) . ?
C1 O1 1.244(7) 1_655 ?
C1 C2 1.525(8) . ?
C1 Ca1 3.167(6) 1_655 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.343(8) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.501(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.419(7) . ?
C7 C13 1.428(6) . ?
C8 C9 1.433(6) . ?
C8 C13 1.448(7) 2_776 ?
C9 C10 1.359(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.413(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.368(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.428(8) 2_776 ?
C12 H12 0.9300 . ?
C13 C12 1.428(8) 2_776 ?
C13 C8 1.448(7) 2_776 ?

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
O3 Ca1 O3 180.0 2_665 . ?
O3 Ca1 O1 85.5(3) 2_665 . ?
O3 Ca1 O1 94.5(3) . . ?
O3 Ca1 O1 94.5(3) 2_665 2_665 ?
O3 Ca1 O1 85.5(3) . 2_665 ?
O1 Ca1 O1 180.0 . 2_665 ?
O3 Ca1 O2 93.43(19) 2_665 2_665 ?
O3 Ca1 O2 86.57(19) . 2_665 ?
O1 Ca1 O2 94.74(15) . 2_665 ?
O1 Ca1 O2 85.26(15) 2_665 2_665 ?
O3 Ca1 O2 86.57(19) 2_665 . ?
O3 Ca1 O2 93.43(19) . . ?
O1 Ca1 O2 85.26(15) . . ?
O1 Ca1 O2 94.74(15) 2_665 . ?
O2 Ca1 O2 180.0 2_665 . ?
O3 Ca1 C1 78.8(2) 2_665 2_765 ?
O3 Ca1 C1 101.2(2) . 2_765 ?
O1 Ca1 C1 160.79(15) . 2_765 ?
O1 Ca1 C1 19.21(15) 2_665 2_765 ?
O2 Ca1 C1 97.16(14) 2_665 2_765 ?
O2 Ca1 C1 82.84(15) . 2_765 ?
O3 Ca1 C1 101.2(2) 2_665 1_455 ?
O3 Ca1 C1 78.8(2) . 1_455 ?
O1 Ca1 C1 19.21(15) . 1_455 ?
O1 Ca1 C1 160.79(15) 2_665 1_455 ?
O2 Ca1 C1 82.84(15) 2_665 1_455 ?
O2 Ca1 C1 97.16(15) . 1_455 ?
C1 Ca1 C1 180.0 2_765 1_455 ?
O3 Ca1 C1 68.08(18) 2_665 . ?
O3 Ca1 C1 111.93(18) . . ?
O1 Ca1 C1 78.52(14) . . ?
O1 Ca1 C1 101.48(14) 2_665 . ?
O2 Ca1 C1 160.59(15) 2_665 . ?
O2 Ca1 C1 19.41(15) . . ?
C1 Ca1 C1 85.34(14) 2_765 . ?
C1 Ca1 C1 94.66(13) 1_455 . ?
O3 Ca1 C1 111.92(18) 2_665 2_665 ?
O3 Ca1 C1 68.07(18) . 2_665 ?
O1 Ca1 C1 101.48(14) . 2_665 ?
O1 Ca1 C1 78.52(14) 2_665 2_665 ?
O2 Ca1 C1 19.41(15) 2_665 2_665 ?
O2 Ca1 C1 160.59(15) . 2_665 ?
C1 Ca1 C1 94.66(13) 2_765 2_665 ?
C1 Ca1 C1 85.34(14) 1_455 2_665 ?
C1 Ca1 C1 180.0 . 2_665 ?
C1 O1 Ca1 123.1(4) 1_455 . ?
C1 O2 Ca1 122.4(4) . . ?
Ca1 O3 H3A 125.8 . . ?
Ca1 O3 H3B 124.9 . . ?
H3A O3 H3B 109.3 . . ?
C5 N4 C4 107.6(4) . . ?
C5 N4 C6 125.7(4) . . ?
C4 N4 C6 126.7(4) . . ?
C5 N6 C3 108.5(4) . . ?
C5 N6 C2 125.8(5) . . ?
C3 N6 C2 125.5(4) . . ?
O1 C1 O2 126.1(5) 1_655 . ?
O1 C1 C2 118.4(5) 1_655 . ?
O2 C1 C2 115.5(5) . . ?
O1 C1 Ca1 37.7(3) 1_655 1_655 ?
O2 C1 Ca1 88.6(3) . 1_655 ?
C2 C1 Ca1 155.7(4) . 1_655 ?
O1 C1 Ca1 125.2(4) 1_655 . ?
O2 C1 Ca1 38.1(3) . . ?
C2 C1 Ca1 102.4(3) . . ?
Ca1 C1 Ca1 94.66(13) 1_655 . ?
N6 C2 C1 113.4(5) . . ?
N6 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
N6 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 N6 106.6(4) . . ?
C4 C3 H3 126.7 . . ?
N6 C3 H3 126.7 . . ?
C3 C4 N4 108.2(5) . . ?
C3 C4 H4 125.9 . . ?
N4 C4 H4 125.9 . . ?
N6 C5 N4 109.1(4) . . ?
N6 C5 H5 125.4 . . ?
N4 C5 H5 125.4 . . ?
N4 C6 C7 111.9(4) . . ?
N4 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
N4 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C8 C7 C13 120.7(4) . . ?
C8 C7 C6 119.1(4) . . ?
C13 C7 C6 120.3(4) . . ?
C7 C8 C9 122.1(4) . . ?
C7 C8 C13 120.6(4) . 2_776 ?
C9 C8 C13 117.3(5) . 2_776 ?
C10 C9 C8 122.1(5) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C9 C10 C11 120.5(5) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 121.7(5) . 2_776 ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 2_776 . ?
C12 C13 C7 122.8(4) 2_776 . ?
C12 C13 C8 118.4(4) 2_776 2_776 ?
C7 C13 C8 118.8(5) . 2_776 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O2 C1 O1 -103.1(6) . . . 1_655 ?
Ca1 O2 C1 C2 77.1(6) . . . . ?
Ca1 O2 C1 Ca1 -99.4(3) . . . 1_655 ?
C5 N6 C2 C1 -95.9(6) . . . . ?
C3 N6 C2 C1 78.7(7) . . . . ?
O1 C1 C2 N6 8.2(8) 1_655 . . . ?
O2 C1 C2 N6 -171.9(5) . . . . ?
Ca1 C1 C2 N6 -0.5(12) 1_655 . . . ?
Ca1 C1 C2 N6 -133.9(4) . . . . ?
C5 N6 C3 C4 -1.3(6) . . . . ?
C2 N6 C3 C4 -176.7(5) . . . . ?
N6 C3 C4 N4 0.8(6) . . . . ?
C5 N4 C4 C3 0.0(6) . . . . ?
C6 N4 C4 C3 -179.1(5) . . . . ?
C3 N6 C5 N4 1.3(6) . . . . ?
C2 N6 C5 N4 176.7(5) . . . . ?
C4 N4 C5 N6 -0.8(6) . . . . ?
C6 N4 C5 N6 178.3(4) . . . . ?
C5 N4 C6 C7 -118.9(5) . . . . ?
C4 N4 C6 C7 60.0(7) . . . . ?
N4 C6 C7 C8 82.8(5) . . . . ?
N4 C6 C7 C13 -97.0(5) . . . . ?
C13 C7 C8 C9 178.9(4) . . . . ?
C6 C7 C8 C9 -0.9(7) . . . . ?
C13 C7 C8 C13 -0.4(8) . . . 2_776 ?
C6 C7 C8 C13 179.8(4) . . . 2_776 ?
C7 C8 C9 C10 179.1(5) . . . . ?
C13 C8 C9 C10 -1.6(8) 2_776 . . . ?
C8 C9 C10 C11 1.4(9) . . . . ?
C9 C10 C11 C12 -1.5(9) . . . . ?
C10 C11 C12 C13 1.8(9) . . . 2_776 ?
C8 C7 C13 C12 -178.9(4) . . . 2_776 ?
C6 C7 C13 C12 0.9(7) . . . 2_776 ?
C8 C7 C13 C8 0.4(8) . . . 2_776 ?
C6 C7 C13 C8 -179.8(4) . . . 2_776 ?

_refine_diff_density_max         1.018
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.133

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_5
_database_code_depnum_ccdc_archive 'CCDC 1024409'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_audit_creation_date             2015-02-07
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        5
_chemical_formula_moiety         
'C54 H66.5 Br0.15 Ca2.5 Cl0.85 N12 Na O17.25, 3(H2 O), 5.5(Br), 1.5(O)'
_chemical_formula_sum            'C54 H72.50 Br5.65 Ca2.50 Cl0.85 N12 Na O21.75'
_chemical_formula_weight         1842.55
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.4574(8)
_cell_length_b                   15.3803(6)
_cell_length_c                   19.4570(11)
_cell_angle_alpha                103.011(4)
_cell_angle_beta                 107.177(5)
_cell_angle_gamma                99.571(4)
_cell_volume                     3899.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13766
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.01
_cell_measurement_theta_min      3.30
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.170
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
'Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1855
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27821
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.700
_diffrn_reflns_theta_max         71.006
_diffrn_reflns_theta_min         3.305
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10621
_reflns_number_total             13719
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00046(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         13719
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0837
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1600P)²+3.2301P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2523
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C3A-C4B
 2.3 with sigma of 0.02
 H15A-H14B
 2.2 with sigma of 0.02
 H9A-H40A
 2.2 with sigma of 0.02
3. Restrained planarity
 C3B, C4B, N3, N4
 with sigma of 0.1
 C3B, C4B, N3, N4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O9: within 1.2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C3B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: Br5(0.15) C3A(0.5) H3AA(0.5) C3B(0.5) H3BA(0.5) C4A(0.5) H4A(0.5)
 C4B(0.5) H4B(0.5) Ca4(0.5) Cl1(0.85) O1B(0.5) O1C(0.25) H1CA(0.25) H1CB(0.25)
 O4(0.5) H4C(0.5) H4D(0.5) O8(0.5) O12(0.5) H12A(0.5) H12B(0.5) O16A(0.5)
 O16B(0.5) Br2A(0.16) Br2B(0.34) Br4B(0.2) Br4C(0.15) Br1B(0.5) Br4A(0.65)
 Br8(0.1) O2A(0.5) Br1A(0.5) O1E(0.5) O2B(0.5) Br7(0.9)
6.a Free rotating group:
 O9(H9A,H9B), O24(H24A,H24B), O15(H15C,H15D)
6.b Rotating group:
 O1C(H1CA,H1CB), O4(H4C,H4D), O10(H10A,H10B), O11(H11A,H11B), O12(H12A,H12B)
6.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C15(H15A,H15B), C16(H16A,H16B), C20(H20A,H20B),
 C26(H26A,H26B), C29(H29A,H29B), C33(H33A,H33B), C43(H43A,H43B), C47(H47A,H47B),
  C49(H49A,H49B), C53(H53A,H53B)
6.d Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C3A(H3AA), C3AA(H3AB), C3B(H3BA), C4A(H4A), C4AA(H4AA), C4B(H4B),
 C17(H17), C18(H18), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C44(H44),
  C45(H45), C46(H46), C50(H50), C51(H51), C52(H52)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br5 Br 0.4902(15) -0.0492(17) 0.6869(12) 0.057(4) Uani 0.15 1 d . . P . .
C1 C 1.0693(4) 0.4200(5) 0.8184(4) 0.0502(13) Uani 1 1 d . . . . .
H1A H 1.0946 0.3695 0.8338 0.075 Uiso 1 1 calc GR . . . .
H1B H 1.1255 0.4731 0.8307 0.075 Uiso 1 1 calc GR . . . .
H1C H 1.0329 0.3999 0.7641 0.075 Uiso 1 1 calc GR . . . .
C1A C 0.6859(4) -0.0888(4) 0.8331(3) 0.0408(11) Uani 1 1 d . . . . .
H1AA H 0.6284 -0.0698 0.8097 0.049 Uiso 1 1 calc R . . . .
C1B C 0.3917(4) -0.0997(4) 0.8656(3) 0.0452(12) Uani 1 1 d . . . . .
C2 C 0.2775(8) -0.2138(7) 0.5682(4) 0.082(2) Uani 1 1 d . . . . .
H2A H 0.3038 -0.1482 0.5732 0.098 Uiso 1 1 calc R . . . .
H2B H 0.2161 -0.2382 0.5231 0.098 Uiso 1 1 calc R . . . .
C2A C 0.3523(7) -0.2648(5) 0.5569(4) 0.068(2) Uani 1 1 d . . . . .
C2B C 0.3806(4) -0.0095(4) 0.8718(3) 0.0460(12) Uani 1 1 d . . . . .
C3 C 0.6533(5) 0.1294(5) 0.9634(4) 0.0506(13) Uani 1 1 d . . . . .
H3A H 0.6531 0.1632 0.9263 0.076 Uiso 1 1 calc GR . . . .
H3B H 0.7137 0.1064 0.9749 0.076 Uiso 1 1 calc GR . . . .
H3C H 0.6524 0.1707 1.0095 0.076 Uiso 1 1 calc GR . . . .
C3A C 0.1922(18) -0.313(2) 0.6347(12) 0.169(19) Uani 0.5 1 d D U P A -1
H3AA H 0.1584 -0.3667 0.5937 0.203 Uiso 0.5 1 calc R . P A -1
C3AA C 0.3066(5) -0.1874(5) 0.7029(4) 0.0540(14) Uani 1 1 d . . . . .
H3AB H 0.3732 -0.1508 0.7195 0.065 Uiso 1 1 calc R . . . .
C3B C 0.1503(16) -0.2053(19) 0.6337(13) 0.121(10) Uani 0.5 1 d . U P A 1
H3BA H 0.0950 -0.2035 0.5934 0.146 Uiso 0.5 1 calc R . P A 1
C4 C 0.6857(11) 0.5527(6) 0.5757(5) 0.107(4) Uani 1 1 d . . . . .
C4A C 0.198(2) -0.301(2) 0.7081(11) 0.158(17) Uani 0.5 1 d . U P A -1
H4A H 0.1662 -0.3427 0.7281 0.190 Uiso 0.5 1 calc R . P A -1
C4AA C 0.5094(5) 0.2896(5) 0.8613(3) 0.0526(14) Uani 1 1 d . . . . .
H4AA H 0.5210 0.3402 0.9038 0.063 Uiso 1 1 calc R . . . .
C4B C 0.1585(17) -0.1952(17) 0.7098(13) 0.107(8) Uani 0.5 1 d D U P A 1
H4B H 0.1099 -0.1835 0.7322 0.129 Uiso 0.5 1 calc R . P A 1
C6 C 0.3000(5) -0.1789(5) 0.8316(4) 0.0555(14) Uani 1 1 d . . . . .
H6A H 0.3151 -0.2318 0.8499 0.067 Uiso 1 1 calc R . . . .
H6B H 0.2459 -0.1606 0.8484 0.067 Uiso 1 1 calc R . . . .
C9 C 0.4662(4) 0.0639(4) 0.9061(3) 0.0434(12) Uani 1 1 d . . . . .
C10 C 0.5613(4) 0.0487(4) 0.9318(3) 0.0439(12) Uani 1 1 d . . . . .
C11 C 0.5706(4) -0.0419(4) 0.9268(3) 0.0427(11) Uani 1 1 d . . . . .
C12 C 0.4864(4) -0.1167(4) 0.8914(3) 0.0437(12) Uani 1 1 d . . . . .
C13 C 0.4980(5) -0.2154(4) 0.8779(4) 0.0541(14) Uani 1 1 d . . . . .
H13A H 0.4446 -0.2538 0.8875 0.081 Uiso 1 1 calc GR . . . .
H13B H 0.5631 -0.2159 0.9119 0.081 Uiso 1 1 calc GR . . . .
H13C H 0.4937 -0.2400 0.8257 0.081 Uiso 1 1 calc GR . . . .
C14 C 0.2795(5) 0.0066(5) 0.8392(4) 0.0539(14) Uani 1 1 d . . . . .
H14A H 0.2341 -0.0505 0.8027 0.081 Uiso 1 1 calc GR . . . .
H14B H 0.2851 0.0548 0.8141 0.081 Uiso 1 1 calc DGR . . . .
H14C H 0.2531 0.0262 0.8796 0.081 Uiso 1 1 calc GR . . . .
C15 C 0.4573(5) 0.1627(4) 0.9150(3) 0.0473(12) Uani 1 1 d . . . . .
H15A H 0.3888 0.1655 0.9134 0.057 Uiso 1 1 calc DR . . . .
H15B H 0.5045 0.2024 0.9648 0.057 Uiso 1 1 calc R . . . .
C16 C 0.6712(5) -0.0588(5) 0.9609(3) 0.0484(13) Uani 1 1 d . . . . .
H16A H 0.7163 -0.0012 0.9985 0.058 Uiso 1 1 calc R . . . .
H16B H 0.6639 -0.1060 0.9874 0.058 Uiso 1 1 calc R . . . .
C17 C 0.8013(5) -0.1235(5) 0.9160(4) 0.0557(14) Uani 1 1 d . . . . .
H17 H 0.8390 -0.1324 0.9618 0.067 Uiso 1 1 calc R . . . .
C18 C 0.8201(5) -0.1413(5) 0.8508(3) 0.0547(14) Uani 1 1 d . . . . .
H18 H 0.8734 -0.1653 0.8422 0.066 Uiso 1 1 calc R . . . .
C20 C 0.7352(5) -0.1291(5) 0.7212(3) 0.0536(14) Uani 1 1 d . . . . .
H20A H 0.7953 -0.1436 0.7117 0.064 Uiso 1 1 calc R . . . .
H20B H 0.7295 -0.0697 0.7107 0.064 Uiso 1 1 calc R . . . .
C21 C 0.6441(8) -0.2037(5) 0.6676(3) 0.072(2) Uani 1 1 d . . . . .
C24 C 0.5195(5) 0.2942(4) 0.7957(4) 0.0524(13) Uani 1 1 d . . . . .
H24 H 0.5405 0.3486 0.7832 0.063 Uiso 1 1 calc R . . . .
C25 C 0.4710(5) 0.1486(5) 0.7882(3) 0.0502(13) Uani 1 1 d . . . . .
H25 H 0.4520 0.0831 0.7705 0.060 Uiso 1 1 calc R . . . .
C26 C 0.4960(6) 0.1748(5) 0.6740(4) 0.0618(17) Uani 1 1 d . . . . .
H26A H 0.4905 0.1077 0.6605 0.074 Uiso 1 1 calc R . . . .
H26B H 0.5617 0.2057 0.6739 0.074 Uiso 1 1 calc R . . . .
C27 C 0.4157(7) 0.1940(5) 0.6149(4) 0.0666(19) Uani 1 1 d . . . . .
C28 C 0.6754(4) 0.0662(4) 0.5826(3) 0.0471(12) Uani 1 1 d . . . . .
C29 C 0.7523(5) 0.1574(5) 0.6016(3) 0.0559(15) Uani 1 1 d . . . . .
H29A H 0.7800 0.1557 0.5606 0.067 Uiso 1 1 calc R . . . .
H29B H 0.7186 0.2084 0.6049 0.067 Uiso 1 1 calc R . . . .
C30 C 0.9096(6) 0.1311(6) 0.6848(5) 0.079(2) Uani 1 1 d . . . . .
H30 H 0.9182 0.0828 0.6490 0.094 Uiso 1 1 calc R . . . .
C31 C 0.9688(6) 0.1687(6) 0.7564(5) 0.073(2) Uani 1 1 d . . . . .
H31 H 1.0293 0.1544 0.7805 0.087 Uiso 1 1 calc R . . . .
C32 C 0.8429(4) 0.2348(4) 0.7355(3) 0.0458(12) Uani 1 1 d . . . . .
H32 H 0.7988 0.2728 0.7419 0.055 Uiso 1 1 calc R . . . .
C33 C 0.9619(4) 0.2851(4) 0.8690(3) 0.0452(12) Uani 1 1 d . . . . .
H33A H 1.0343 0.2896 0.8906 0.054 Uiso 1 1 calc R . . . .
H33B H 0.9275 0.2512 0.8958 0.054 Uiso 1 1 calc R . . . .
C34 C 0.9453(4) 0.3808(4) 0.8818(3) 0.0409(11) Uani 1 1 d . . . . .
C35 C 0.8762(4) 0.4042(4) 0.9159(3) 0.0414(11) Uani 1 1 d . . . . .
C36 C 0.8700(4) 0.4965(4) 0.9350(3) 0.0396(11) Uani 1 1 d . . . . .
C37 C 0.9247(4) 0.5627(4) 0.9138(3) 0.0409(11) Uani 1 1 d . . . . .
C38 C 0.9875(4) 0.5367(4) 0.8739(3) 0.0418(11) Uani 1 1 d . . . . .
C39 C 0.9995(4) 0.4473(4) 0.8596(3) 0.0422(11) Uani 1 1 d . . . . .
C40 C 0.8093(4) 0.3314(4) 0.9325(3) 0.0446(12) Uani 1 1 d . . . . .
H40A H 0.7954 0.2719 0.8951 0.067 Uiso 1 1 calc DGR . . . .
H40B H 0.7464 0.3484 0.9304 0.067 Uiso 1 1 calc GR . . . .
H40C H 0.8428 0.3267 0.9828 0.067 Uiso 1 1 calc GR . . . .
C42 C 0.9165(5) 0.6612(4) 0.9323(4) 0.0497(13) Uani 1 1 d . . . . .
H42A H 0.8977 0.6796 0.8860 0.075 Uiso 1 1 calc GR . . . .
H42B H 0.9810 0.7015 0.9672 0.075 Uiso 1 1 calc GR . . . .
H42C H 0.8653 0.6664 0.9556 0.075 Uiso 1 1 calc GR . . . .
C43 C 0.8011(4) 0.5229(4) 0.9771(3) 0.0404(11) Uani 1 1 d . . . . .
H43A H 0.7854 0.4752 1.0015 0.049 Uiso 1 1 calc R . . . .
H43B H 0.8355 0.5820 1.0170 0.049 Uiso 1 1 calc R . . . .
C44 C 0.6247(4) 0.5454(4) 0.9461(3) 0.0461(12) Uani 1 1 d . . . . .
H44 H 0.6150 0.5412 0.9916 0.055 Uiso 1 1 calc R . . . .
C45 C 0.5608(4) 0.5652(4) 0.8884(3) 0.0476(12) Uani 1 1 d . . . . .
H45 H 0.4975 0.5770 0.8855 0.057 Uiso 1 1 calc R . . . .
C46 C 0.6928(4) 0.5441(4) 0.8593(3) 0.0455(12) Uani 1 1 d . . . . .
H46 H 0.7382 0.5386 0.8328 0.055 Uiso 1 1 calc R . . . .
C47 C 0.5694(5) 0.5848(5) 0.7629(4) 0.0555(14) Uani 1 1 d . . . . .
H47A H 0.6245 0.5921 0.7426 0.067 Uiso 1 1 calc R . . . .
H47B H 0.5505 0.6443 0.7721 0.067 Uiso 1 1 calc R . . . .
C48 C 0.4812(6) 0.5122(5) 0.7050(4) 0.0571(15) Uani 1 1 d . . . . .
C49 C 1.0387(4) 0.6070(5) 0.8449(3) 0.0488(13) Uani 1 1 d . . . . .
H49A H 1.0586 0.6687 0.8819 0.059 Uiso 1 1 calc R . . . .
H49B H 1.0999 0.5911 0.8388 0.059 Uiso 1 1 calc R . . . .
C50 C 0.9694(9) 0.6909(7) 0.7482(5) 0.088(3) Uani 1 1 d . . . B -1
H50 H 1.0118 0.7505 0.7760 0.106 Uiso 1 1 calc R . . B -1
C51 C 0.8990(8) 0.6690(7) 0.6814(6) 0.086(3) Uani 1 1 d . . . B -1
H51 H 0.8786 0.7097 0.6531 0.104 Uiso 1 1 calc R . . B -1
C52 C 0.8989(4) 0.5436(4) 0.7188(3) 0.0475(12) Uani 1 1 d . . . . .
H52 H 0.8778 0.4835 0.7225 0.057 Uiso 1 1 calc R . . . .
C53 C 0.7770(6) 0.5157(6) 0.5904(4) 0.070(2) Uani 1 1 d . . . . .
H53A H 0.7585 0.4521 0.5936 0.084 Uiso 1 1 calc R . . . .
H53B H 0.8008 0.5124 0.5474 0.084 Uiso 1 1 calc R . . . .
Ca1 Ca 0.53102(9) -0.10460(8) 0.54550(6) 0.0449(3) Uani 1 1 d . . . . .
Ca3 Ca 0.49413(13) 0.37566(10) 0.43075(7) 0.0644(4) Uani 1 1 d . . . . .
Ca4 Ca 0.2843(3) 0.2512(2) 0.49459(17) 0.0783(10) Uani 0.5 1 d . . P C .
Cl1 Cl 0.5100(6) -0.0521(7) 0.6820(4) 0.0512(11) Uani 0.85 1 d . . P . .
N1 N 0.4937(4) 0.2047(4) 0.7499(3) 0.0502(11) Uani 1 1 d . . . . .
N2 N 0.4792(4) 0.1988(3) 0.8552(3) 0.0436(10) Uani 1 1 d . . . . .
N3 N 0.2523(6) -0.2198(8) 0.6324(4) 0.099(3) Uani 1 1 d . . . . .
N4 N 0.2652(5) -0.2077(7) 0.7491(4) 0.092(3) Uani 1 1 d . . . . .
N5 N 0.7176(4) -0.0903(3) 0.9036(3) 0.0444(10) Uani 1 1 d . . . . .
N6 N 0.7486(4) -0.1187(4) 0.8002(3) 0.0462(10) Uani 1 1 d . . . . .
N7 N 0.9252(3) 0.2327(3) 0.7892(3) 0.0455(10) Uani 1 1 d . . . . .
N8 N 0.8340(4) 0.1753(4) 0.6724(3) 0.0535(12) Uani 1 1 d . . . . .
N9 N 0.7066(3) 0.5326(3) 0.9261(3) 0.0414(9) Uani 1 1 d . . . . .
N10 N 0.6058(4) 0.5647(4) 0.8344(3) 0.0471(10) Uani 1 1 d . . . . .
N11 N 0.9708(5) 0.6097(5) 0.7712(3) 0.0712(18) Uani 1 1 d . . . . .
N12 N 0.8600(5) 0.5717(5) 0.6604(3) 0.076(2) Uani 1 1 d . . . . .
Na2 Na 0.28501(14) 0.33807(13) 0.70187(10) 0.0355(4) Uani 1 1 d . . . . .
O1A O 0.5867(6) -0.1658(4) 0.4508(3) 0.086(2) Uani 1 1 d . . . . .
O1B O 0.2605(7) 0.3800(6) 0.5782(4) 0.0510(19) Uani 0.5 1 d . . P C 1
O1C O 0.1700(12) 0.1070(13) 0.4215(10) 0.053(4) Uani 0.25 1 d . . P C .
H1CA H 0.0943 0.0881 0.4284 0.080 Uiso 0.25 1 d GR . P . .
H1CB H 0.1924 0.0401 0.4262 0.080 Uiso 0.25 1 d GR . P . .
O2C O 0.4360(4) 0.4521(4) 0.7238(3) 0.0624(11) Uani 1 1 d . . . . .
O2D O 0.6213(5) -0.2076(4) 0.5984(3) 0.0726(15) Uani 1 1 d . . . . .
O3 O 0.4056(5) -0.2398(4) 0.5211(3) 0.0794(17) Uani 1 1 d . . . . .
O4 O 0.1151(10) 0.2806(11) 0.6472(10) 0.102(5) Uani 0.5 1 d . . P C .
H4C H 0.0723 0.2238 0.5826 0.152 Uiso 0.5 1 d GR . P . .
H4D H 0.0551 0.3303 0.6338 0.152 Uiso 0.5 1 d GR . P . .
O5 O 0.6965(4) 0.0079(4) 0.6129(3) 0.0745(15) Uani 1 1 d . . . . .
O6 O 0.4071(4) -0.0558(4) 0.4674(3) 0.0692(13) Uani 1 1 d . . . . .
O7 O 0.3583(5) 0.2409(5) 0.6337(3) 0.0800(16) Uani 1 1 d . . . . .
O8 O 0.3472(5) 0.3888(5) 0.5850(4) 0.0370(14) Uani 0.5 1 d . . P C -1
O10 O 0.2611(6) 0.2036(5) 0.7456(4) 0.095(2) Uani 1 1 d . . . . .
H10A H 0.2683 0.2048 0.7922 0.143 Uiso 1 1 d GR . . . .
H10B H 0.2438 0.1463 0.7175 0.143 Uiso 1 1 d GR . . . .
O11 O 0.3190(5) 0.3887(5) 0.8357(4) 0.0839(16) Uani 1 1 d . . . . .
H11A H 0.3117 0.3512 0.8649 0.126 Uiso 1 1 d GR . . . .
H11B H 0.3411 0.4482 0.8650 0.126 Uiso 1 1 d GR . . . .
O12 O 0.2323(10) 0.4808(8) 0.7270(6) 0.072(3) Uani 0.5 1 d . . P C .
H12A H 0.2715 0.5358 0.7616 0.108 Uiso 0.5 1 d GR . P . .
H12B H 0.1700 0.4886 0.7035 0.108 Uiso 0.5 1 d GR . P . .
O13 O 0.4731(6) 0.3582(4) 0.5471(3) 0.0780(16) Uani 1 1 d . . . . .
O14 O 0.6103(5) 0.5070(4) 0.5266(3) 0.0805(16) Uani 1 1 d . . . . .
O16A O 0.6644(8) 0.6116(8) 0.6343(6) 0.067(2) Uani 0.5 1 d . . P D 1
O16B O 0.7195(18) 0.6407(11) 0.5884(10) 0.138(9) Uani 0.5 1 d . . P D -1
O17 O 0.3598(6) -0.3304(4) 0.5834(4) 0.0895(18) Uani 1 1 d . . . . .
O18 O 0.5951(7) -0.2557(4) 0.6914(3) 0.109(3) Uani 1 1 d . . . . .
O19 O 0.4576(6) 0.5213(4) 0.6393(3) 0.087(2) Uani 1 1 d . . . . .
O9 O 0.7010(4) 0.1229(4) 0.7902(3) 0.0693(13) Uani 1 1 d . U . . .
H9A H 0.6731 0.1546 0.8174 0.104 Uiso 1 1 d DG . . . .
H9B H 0.6608 0.0688 0.7652 0.104 Uiso 1 1 d G . . . .
Br2A Br 0.2306(16) 0.0040(12) 0.6215(14) 0.160(9) Uani 0.16 1 d . . P E -1
Br2B Br 0.2084(7) -0.0054(4) 0.6313(3) 0.142(3) Uani 0.34 1 d . . P F 1
O24 O 0.8680(5) 0.0930(4) 0.8959(4) 0.0787(15) Uani 1 1 d . . . . .
H24A H 0.8921 0.0995 0.9438 0.118 Uiso 1 1 d G . . . .
H24B H 0.9085 0.0732 0.8744 0.118 Uiso 1 1 d G . . . .
O15 O 1.0350(6) 0.0402(6) 0.8653(6) 0.106(2) Uani 1 1 d . . . . .
H15C H 1.0809 0.0919 0.8850 0.158 Uiso 1 1 d G . . . .
H15D H 1.0534 0.0004 0.8886 0.158 Uiso 1 1 d G . . . .
Br4B Br 0.9965(8) 0.3959(9) 0.5316(5) 0.157(4) Uani 0.2 1 d . . P G 1
Br4C Br 1.0167(16) 0.4578(12) 0.6086(10) 0.173(6) Uani 0.15 1 d . . P H 3
Br1B Br 0.2254(4) 0.2415(4) 0.9137(2) 0.0466(6) Uani 0.5 1 d . . P I 1
Br4A Br 0.93795(14) 0.34918(16) 0.59471(10) 0.1043(6) Uani 0.65 1 d . . P G -1
Br8 Br 0.9233(6) 0.1527(6) 1.1205(5) 0.060(2) Uani 0.1 1 d . . P J 1
O2A O 0.0288(15) 0.0937(14) 0.2832(11) 0.112(6) Uani 0.5 1 d . . P K 1
Br1A Br 0.2158(4) 0.2320(4) 0.9294(3) 0.0639(9) Uani 0.5 1 d . . P L -1
O1E O 0.9358(18) 0.0975(19) 0.5128(10) 0.145(9) Uani 0.5 1 d . . P M -1
Br3 Br 0.67844(6) 0.38418(6) 0.69691(4) 0.0650(2) Uani 1 1 d . . . . .
O2B O -0.0191(18) 0.083(2) 0.3078(16) 0.181(15) Uani 0.5 1 d . . P K -1
Br6 Br 0.67282(5) 0.39360(5) 1.08163(4) 0.0558(2) Uani 1 1 d . . . . .
Br7 Br 0.90662(6) 0.12898(7) 1.07669(8) 0.0659(3) Uani 0.9 1 d . . P J -1


_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
Br5 Ca1 2.953(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C39 1.518(8) . ?
C1A H1AA 0.9500 . ?
C1A N5 1.318(7) . ?
C1A N6 1.338(7) . ?
C1B C2B 1.406(9) . ?
C1B C6 1.503(9) . ?
C1B C12 1.402(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C2A 1.475(14) . ?
C2 N3 1.418(11) . ?
C2A Ca3 3.004(10) 2_656 ?
C2A O3 1.252(9) . ?
C2A O17 1.238(10) . ?
C2B C9 1.400(9) . ?
C2B C14 1.498(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 C10 1.520(8) . ?
C3A H3AA 0.9500 . ?
C3A C3B 1.85(4) . ?
C3A C4A 1.37(3) . ?
C3A N3 1.56(3) . ?
C3AA H3AB 0.9500 . ?
C3AA N3 1.293(10) . ?
C3AA N4 1.282(9) . ?
C3B H3BA 0.9500 . ?
C3B C4B 1.42(3) . ?
C3B N3 1.53(3) . ?
C4 C53 1.499(16) . ?
C4 Ca3 2.969(13) 2_666 ?
C4 O14 1.193(12) . ?
C4 O16A 1.433(16) . ?
C4 O16B 1.30(2) . ?
C4A H4A 0.9500 . ?
C4A C4B 1.80(5) . ?
C4A N4 1.48(2) . ?
C4AA H4AA 0.9500 . ?
C4AA C24 1.342(9) . ?
C4AA N2 1.360(9) . ?
C4B H4B 0.9500 . ?
C4B N4 1.57(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 N4 1.468(9) . ?
C9 C10 1.397(9) . ?
C9 C15 1.521(8) . ?
C10 C11 1.405(8) . ?
C11 C12 1.401(8) . ?
C11 C16 1.502(8) . ?
C12 C13 1.529(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N2 1.488(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 N5 1.495(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.353(9) . ?
C17 N5 1.367(8) . ?
C18 H18 0.9500 . ?
C18 N6 1.353(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.512(11) . ?
C20 N6 1.460(8) . ?
C21 Ca3 2.891(8) 2_656 ?
C21 O2D 1.274(8) . ?
C21 O18 1.236(11) . ?
C24 H24 0.9500 . ?
C24 N1 1.382(9) . ?
C25 H25 0.9500 . ?
C25 N1 1.323(8) . ?
C25 N2 1.317(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.495(11) . ?
C26 N1 1.456(8) . ?
C27 Ca4 2.953(8) . ?
C27 O1A 1.241(8) 2_656 ?
C27 O7 1.266(10) . ?
C28 C29 1.531(9) . ?
C28 Ca1 2.866(6) . ?
C28 O5 1.212(8) . ?
C28 O6 1.255(8) 2_656 ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 N8 1.459(8) . ?
C30 H30 0.9500 . ?
C30 C31 1.332(11) . ?
C30 N8 1.370(10) . ?
C31 H31 0.9500 . ?
C31 N7 1.392(9) . ?
C32 H32 0.9500 . ?
C32 N7 1.343(8) . ?
C32 N8 1.312(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.509(8) . ?
C33 N7 1.465(8) . ?
C34 C35 1.404(8) . ?
C34 C39 1.407(8) . ?
C35 C36 1.409(8) . ?
C35 C40 1.510(7) . ?
C36 C37 1.395(8) . ?
C36 C43 1.515(7) . ?
C37 C38 1.408(8) . ?
C37 C42 1.510(9) . ?
C38 C39 1.390(9) . ?
C38 C49 1.514(8) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 N9 1.484(7) . ?
C44 H44 0.9500 . ?
C44 C45 1.357(9) . ?
C44 N9 1.382(7) . ?
C45 H45 0.9500 . ?
C45 N10 1.388(7) . ?
C46 H46 0.9500 . ?
C46 N9 1.312(7) . ?
C46 N10 1.326(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.501(10) . ?
C47 N10 1.457(8) . ?
C48 O2C 1.229(9) . ?
C48 O19 1.268(9) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 N11 1.493(9) . ?
C50 H50 0.9500 . ?
C50 C51 1.323(14) . ?
C50 N11 1.419(12) . ?
C51 H51 0.9500 . ?
C51 N12 1.425(12) . ?
C52 H52 0.9500 . ?
C52 N11 1.308(9) . ?
C52 N12 1.312(9) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 N12 1.483(10) . ?
Ca1 Ca1 4.108(2) 2_656 ?
Ca1 Ca3 4.2648(18) 2_656 ?
Ca1 Ca4 3.907(4) 2_656 ?
Ca1 Cl1 2.719(7) . ?
Ca1 O1A 2.297(5) . ?
Ca1 O2D 2.429(5) . ?
Ca1 O3 2.373(5) . ?
Ca1 O5 2.487(5) . ?
Ca1 O6 2.575(5) 2_656 ?
Ca1 O6 2.331(5) . ?
Ca3 C2A 3.004(10) 2_656 ?
Ca3 C4 2.969(13) 2_666 ?
Ca3 C21 2.891(8) 2_656 ?
Ca3 O2D 2.671(6) 2_656 ?
Ca3 O3 2.903(8) 2_656 ?
Ca3 O13 2.437(5) . ?
Ca3 O14 2.682(7) 2_666 ?
Ca3 O14 2.389(6) . ?
Ca3 O16A 2.333(10) 2_666 ?
Ca3 O17 2.401(8) 2_656 ?
Ca3 O18 2.478(6) 2_656 ?
Ca3 O19 2.454(6) 2_666 ?
Ca4 Ca1 3.907(4) 2_656 ?
Ca4 Na2 3.949(3) . ?
Ca4 O1A 2.570(7) 2_656 ?
Ca4 O1B 2.408(9) . ?
Ca4 O1C 2.376(19) . ?
Ca4 O2D 2.608(7) 2_656 ?
Ca4 O7 2.652(6) . ?
Ca4 O8 2.267(8) . ?
Ca4 O13 2.704(8) . ?
Na2 O1B 2.570(8) . ?
Na2 O2C 2.421(6) . ?
Na2 O4 2.293(13) . ?
Na2 O7 2.363(6) . ?
Na2 O8 2.891(7) . ?
Na2 O10 2.418(7) . ?
Na2 O11 2.416(7) . ?
Na2 O12 2.436(10) . ?
O1A C27 1.241(8) 2_656 ?
O1A Ca4 2.570(7) 2_656 ?
O1B O8 1.202(11) . ?
O1C H1CA 1.1409 . ?
O1C H1CB 1.1432 . ?
O2D Ca3 2.671(6) 2_656 ?
O2D Ca4 2.608(7) 2_656 ?
O3 Ca3 2.903(8) 2_656 ?
O4 H4C 1.2619 . ?
O4 H4D 1.2573 . ?
O6 C28 1.255(8) 2_656 ?
O6 Ca1 2.575(5) 2_656 ?
O10 H10A 0.8766 . ?
O10 H10B 0.8767 . ?
O11 H11A 0.9092 . ?
O11 H11B 0.9089 . ?
O12 H12A 0.9218 . ?
O12 H12B 0.9232 . ?
O14 Ca3 2.682(7) 2_666 ?
O16A Ca3 2.333(10) 2_666 ?
O16A O16B 1.45(3) . ?
O17 Ca3 2.401(8) 2_656 ?
O18 Ca3 2.478(6) 2_656 ?
O19 Ca3 2.454(6) 2_666 ?
O9 H9A 0.8701 . ?
O9 H9B 0.8700 . ?
O24 H24A 0.8689 . ?
O24 H24B 0.8704 . ?
O15 H15C 0.8701 . ?
O15 H15D 0.8705 . ?
Br4B Br4A 1.884(12) . ?
Br8 Br7 0.792(8) . ?
O2A O2B 0.96(3) . ?

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
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C39 C1 H1A 109.5 . . ?
C39 C1 H1B 109.5 . . ?
C39 C1 H1C 109.5 . . ?
N5 C1A H1AA 125.8 . . ?
N5 C1A N6 108.4(5) . . ?
N6 C1A H1AA 125.8 . . ?
C2B C1B C6 119.1(6) . . ?
C12 C1B C2B 121.1(5) . . ?
C12 C1B C6 119.8(6) . . ?
H2A C2 H2B 107.7 . . ?
C2A C2 H2A 108.9 . . ?
C2A C2 H2B 108.9 . . ?
N3 C2 H2A 108.9 . . ?
N3 C2 H2B 108.9 . . ?
N3 C2 C2A 113.5(9) . . ?
C2 C2A Ca3 166.3(5) . 2_656 ?
O3 C2A C2 118.7(8) . . ?
O3 C2A Ca3 73.3(6) . 2_656 ?
O17 C2A C2 118.6(7) . . ?
O17 C2A Ca3 49.9(5) . 2_656 ?
O17 C2A O3 122.7(9) . . ?
C1B C2B C14 120.2(6) . . ?
C9 C2B C1B 118.6(5) . . ?
C9 C2B C14 121.1(6) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C3 H3A 109.5 . . ?
C10 C3 H3B 109.5 . . ?
C10 C3 H3C 109.5 . . ?
C3B C3A H3AA 119.3 . . ?
C4A C3A H3AA 126.9 . . ?
C4A C3A C3B 91(2) . . ?
C4A C3A N3 106.1(15) . . ?
N3 C3A H3AA 126.9 . . ?
N3 C3A C3B 52.5(13) . . ?
N3 C3AA H3AB 122.0 . . ?
N4 C3AA H3AB 122.0 . . ?
N4 C3AA N3 116.0(7) . . ?
C3A C3B H3BA 121.3 . . ?
C4B C3B C3A 86.8(15) . . ?
C4B C3B H3BA 128.3 . . ?
C4B C3B N3 103.3(17) . . ?
N3 C3B C3A 53.9(12) . . ?
N3 C3B H3BA 128.3 . . ?
C53 C4 Ca3 171.4(7) . 2_666 ?
O14 C4 C53 119.3(8) . . ?
O14 C4 Ca3 64.5(7) . 2_666 ?
O14 C4 O16A 110.7(12) . . ?
O14 C4 O16B 124.1(10) . . ?
O16A C4 C53 122.5(7) . . ?
O16A C4 Ca3 50.4(6) . 2_666 ?
O16B C4 C53 104.9(15) . . ?
O16B C4 Ca3 76.9(13) . 2_666 ?
O16B C4 O16A 64.0(13) . . ?
C3A C4A H4A 127.7 . . ?
C3A C4A C4B 90(3) . . ?
C3A C4A N4 104.7(17) . . ?
C4B C4A H4A 116.9 . . ?
N4 C4A H4A 127.7 . . ?
N4 C4A C4B 56.1(15) . . ?
C24 C4AA H4AA 126.5 . . ?
C24 C4AA N2 106.9(6) . . ?
N2 C4AA H4AA 126.5 . . ?
C3B C4B C4A 91.7(14) . . ?
C3B C4B H4B 127.4 . . ?
C3B C4B N4 105.2(15) . . ?
C4A C4B H4B 119.2 . . ?
N4 C4B C4A 51.5(11) . . ?
N4 C4B H4B 127.4 . . ?
C1B C6 H6A 109.1 . . ?
C1B C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N4 C6 C1B 112.3(5) . . ?
N4 C6 H6A 109.1 . . ?
N4 C6 H6B 109.1 . . ?
C2B C9 C15 120.3(5) . . ?
C10 C9 C2B 121.3(5) . . ?
C10 C9 C15 118.4(5) . . ?
C9 C10 C3 119.9(5) . . ?
C9 C10 C11 119.2(5) . . ?
C11 C10 C3 120.9(5) . . ?
C10 C11 C16 119.9(5) . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 C16 119.5(5) . . ?
C1B C12 C13 120.4(5) . . ?
C11 C12 C1B 119.1(5) . . ?
C11 C12 C13 120.4(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C2B C14 H14A 109.5 . . ?
C2B C14 H14B 109.5 . . ?
C2B C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.2 . . ?
C9 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N2 C15 C9 112.0(4) . . ?
N2 C15 H15A 109.2 . . ?
N2 C15 H15B 109.2 . . ?
C11 C16 H16A 109.1 . . ?
C11 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
N5 C16 C11 112.6(4) . . ?
N5 C16 H16A 109.1 . . ?
N5 C16 H16B 109.1 . . ?
C18 C17 H17 126.5 . . ?
C18 C17 N5 107.0(5) . . ?
N5 C17 H17 126.5 . . ?
C17 C18 H18 126.4 . . ?
C17 C18 N6 107.2(6) . . ?
N6 C18 H18 126.4 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
N6 C20 H20A 108.9 . . ?
N6 C20 H20B 108.9 . . ?
N6 C20 C21 113.4(5) . . ?
C20 C21 Ca3 165.2(6) . 2_656 ?
O2D C21 C20 116.0(7) . . ?
O2D C21 Ca3 67.2(4) . 2_656 ?
O18 C21 C20 120.7(6) . . ?
O18 C21 Ca3 58.4(4) . 2_656 ?
O18 C21 O2D 123.3(8) . . ?
C4AA C24 H24 126.5 . . ?
C4AA C24 N1 107.0(5) . . ?
N1 C24 H24 126.5 . . ?
N1 C25 H25 125.8 . . ?
N2 C25 H25 125.8 . . ?
N2 C25 N1 108.4(6) . . ?
H26A C26 H26B 107.5 . . ?
C27 C26 H26A 108.5 . . ?
C27 C26 H26B 108.5 . . ?
N1 C26 H26A 108.5 . . ?
N1 C26 H26B 108.5 . . ?
N1 C26 C27 114.9(6) . . ?
C26 C27 Ca4 170.6(6) . . ?
O1A C27 C26 116.3(7) 2_656 . ?
O1A C27 Ca4 60.1(4) 2_656 . ?
O1A C27 O7 123.7(7) 2_656 . ?
O7 C27 C26 119.8(6) . . ?
O7 C27 Ca4 63.9(4) . . ?
C29 C28 Ca1 179.4(4) . . ?
O5 C28 C29 120.6(6) . . ?
O5 C28 Ca1 59.8(3) . . ?
O5 C28 O6 123.7(6) . 2_656 ?
O6 C28 C29 115.7(6) 2_656 . ?
O6 C28 Ca1 63.9(3) 2_656 . ?
C28 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
N8 C29 C28 112.2(5) . . ?
N8 C29 H29A 109.2 . . ?
N8 C29 H29B 109.2 . . ?
C31 C30 H30 126.4 . . ?
C31 C30 N8 107.3(6) . . ?
N8 C30 H30 126.4 . . ?
C30 C31 H31 126.4 . . ?
C30 C31 N7 107.1(6) . . ?
N7 C31 H31 126.4 . . ?
N7 C32 H32 125.9 . . ?
N8 C32 H32 125.9 . . ?
N8 C32 N7 108.2(5) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
N7 C33 H33A 109.0 . . ?
N7 C33 H33B 109.0 . . ?
N7 C33 C34 112.9(5) . . ?
C35 C34 C33 120.4(5) . . ?
C35 C34 C39 119.7(5) . . ?
C39 C34 C33 119.9(5) . . ?
C34 C35 C36 119.4(5) . . ?
C34 C35 C40 120.5(5) . . ?
C36 C35 C40 120.1(5) . . ?
C35 C36 C43 119.4(5) . . ?
C37 C36 C35 120.5(5) . . ?
C37 C36 C43 120.0(5) . . ?
C36 C37 C38 119.3(5) . . ?
C36 C37 C42 120.9(5) . . ?
C38 C37 C42 119.8(5) . . ?
C37 C38 C49 118.7(5) . . ?
C39 C38 C37 120.5(5) . . ?
C39 C38 C49 120.8(5) . . ?
C34 C39 C1 119.4(5) . . ?
C38 C39 C1 120.4(5) . . ?
C38 C39 C34 120.1(5) . . ?
C35 C40 H40A 109.5 . . ?
C35 C40 H40B 109.5 . . ?
C35 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C37 C42 H42A 109.5 . . ?
C37 C42 H42B 109.5 . . ?
C37 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C36 C43 H43A 109.3 . . ?
C36 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
N9 C43 C36 111.6(4) . . ?
N9 C43 H43A 109.3 . . ?
N9 C43 H43B 109.3 . . ?
C45 C44 H44 126.6 . . ?
C45 C44 N9 106.9(5) . . ?
N9 C44 H44 126.6 . . ?
C44 C45 H45 126.7 . . ?
C44 C45 N10 106.7(5) . . ?
N10 C45 H45 126.7 . . ?
N9 C46 H46 125.2 . . ?
N9 C46 N10 109.6(5) . . ?
N10 C46 H46 125.2 . . ?
H47A C47 H47B 107.6 . . ?
C48 C47 H47A 108.7 . . ?
C48 C47 H47B 108.7 . . ?
N10 C47 H47A 108.7 . . ?
N10 C47 H47B 108.7 . . ?
N10 C47 C48 114.0(5) . . ?
O2C C48 C47 119.7(6) . . ?
O2C C48 O19 125.2(7) . . ?
O19 C48 C47 115.0(7) . . ?
C38 C49 H49A 109.5 . . ?
C38 C49 H49B 109.5 . . ?
H49A C49 H49B 108.1 . . ?
N11 C49 C38 110.8(5) . . ?
N11 C49 H49A 109.5 . . ?
N11 C49 H49B 109.5 . . ?
C51 C50 H50 126.0 . . ?
C51 C50 N11 108.0(8) . . ?
N11 C50 H50 126.0 . . ?
C50 C51 H51 127.1 . . ?
C50 C51 N12 105.9(8) . . ?
N12 C51 H51 127.1 . . ?
N11 C52 H52 124.7 . . ?
N11 C52 N12 110.6(6) . . ?
N12 C52 H52 124.7 . . ?
C4 C53 H53A 108.8 . . ?
C4 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
N12 C53 C4 113.7(8) . . ?
N12 C53 H53A 108.8 . . ?
N12 C53 H53B 108.8 . . ?
Br5 Ca1 Ca1 101.4(5) . 2_656 ?
Br5 Ca1 Ca3 88.0(5) . 2_656 ?
Br5 Ca1 Ca4 127.4(5) . 2_656 ?
C28 Ca1 Br5 92.6(5) . . ?
C28 Ca1 Ca1 57.15(13) . 2_656 ?
C28 Ca1 Ca3 141.59(13) . 2_656 ?
C28 Ca1 Ca4 92.86(14) . 2_656 ?
Ca1 Ca1 Ca3 159.36(5) 2_656 2_656 ?
Ca4 Ca1 Ca1 124.87(6) 2_656 2_656 ?
Ca4 Ca1 Ca3 57.97(6) 2_656 2_656 ?
Cl1 Ca1 Br5 4.8(6) . . ?
Cl1 Ca1 C28 90.1(2) . . ?
Cl1 Ca1 Ca1 103.5(2) . 2_656 ?
Cl1 Ca1 Ca3 87.3(2) . 2_656 ?
Cl1 Ca1 Ca4 123.4(2) . 2_656 ?
O1A Ca1 Br5 166.4(5) . . ?
O1A Ca1 C28 89.5(2) . . ?
O1A Ca1 Ca1 91.01(14) . 2_656 ?
O1A Ca1 Ca3 82.12(15) . 2_656 ?
O1A Ca1 Ca4 39.08(15) . 2_656 ?
O1A Ca1 Cl1 162.4(2) . . ?
O1A Ca1 O2D 78.74(19) . . ?
O1A Ca1 O3 94.9(2) . . ?
O1A Ca1 O5 89.9(3) . . ?
O1A Ca1 O6 93.8(2) . . ?
O1A Ca1 O6 88.2(2) . 2_656 ?
O2D Ca1 Br5 87.8(5) . . ?
O2D Ca1 C28 106.5(2) . . ?
O2D Ca1 Ca1 161.19(18) . 2_656 ?
O2D Ca1 Ca3 35.08(16) . 2_656 ?
O2D Ca1 Ca4 40.83(14) . 2_656 ?
O2D Ca1 Cl1 84.5(2) . . ?
O2D Ca1 O5 82.2(2) . . ?
O2D Ca1 O6 131.4(2) . 2_656 ?
O3 Ca1 Br5 83.3(5) . . ?
O3 Ca1 C28 175.48(19) . . ?
O3 Ca1 Ca1 121.72(19) . 2_656 ?
O3 Ca1 Ca3 40.50(19) . 2_656 ?
O3 Ca1 Ca4 91.15(19) . 2_656 ?
O3 Ca1 Cl1 85.9(2) . . ?
O3 Ca1 O2D 75.3(3) . . ?
O3 Ca1 O5 155.6(2) . . ?
O3 Ca1 O6 153.0(2) . 2_656 ?
O5 Ca1 Br5 86.4(5) . . ?
O5 Ca1 C28 24.91(18) . . ?
O5 Ca1 Ca1 82.04(13) . 2_656 ?
O5 Ca1 Ca3 117.20(13) . 2_656 ?
O5 Ca1 Ca4 77.64(18) . 2_656 ?
O5 Ca1 Cl1 82.4(2) . . ?
O5 Ca1 O6 50.87(16) . 2_656 ?
O6 Ca1 Br5 99.6(5) . . ?
O6 Ca1 Br5 99.5(5) 2_656 . ?
O6 Ca1 C28 92.12(18) . . ?
O6 Ca1 C28 25.98(17) 2_656 . ?
O6 Ca1 Ca1 35.03(12) . 2_656 ?
O6 Ca1 Ca1 31.30(11) 2_656 2_656 ?
O6 Ca1 Ca3 125.67(13) . 2_656 ?
O6 Ca1 Ca3 164.89(14) 2_656 2_656 ?
O6 Ca1 Ca4 107.54(15) 2_656 2_656 ?
O6 Ca1 Ca4 132.45(17) . 2_656 ?
O6 Ca1 Cl1 103.8(2) . . ?
O6 Ca1 Cl1 99.0(3) 2_656 . ?
O6 Ca1 O2D 159.69(19) . . ?
O6 Ca1 O3 86.7(2) . . ?
O6 Ca1 O5 116.93(18) . . ?
O6 Ca1 O6 66.33(19) . 2_656 ?
C4 Ca3 C2A 166.4(3) 2_666 2_656 ?
C21 Ca3 C2A 84.5(2) 2_656 2_656 ?
C21 Ca3 C4 86.0(3) 2_656 2_666 ?
C21 Ca3 O3 77.54(19) 2_656 2_656 ?
O2D Ca3 C2A 79.5(2) 2_656 2_656 ?
O2D Ca3 C4 87.7(3) 2_656 2_666 ?
O2D Ca3 C21 26.10(17) 2_656 2_656 ?
O2D Ca3 O3 63.37(17) 2_656 2_656 ?
O2D Ca3 O14 105.3(2) 2_656 2_666 ?
O3 Ca3 C2A 24.39(18) 2_656 2_656 ?
O3 Ca3 C4 142.9(3) 2_656 2_666 ?
O13 Ca3 C2A 91.9(2) . 2_656 ?
O13 Ca3 C4 79.6(3) . 2_666 ?
O13 Ca3 C21 96.9(2) . 2_656 ?
O13 Ca3 O2D 71.56(17) . 2_656 ?
O13 Ca3 O3 69.87(18) . 2_656 ?
O13 Ca3 O14 71.3(2) . 2_666 ?
O13 Ca3 O18 122.0(2) . 2_656 ?
O13 Ca3 O19 148.30(19) . 2_666 ?
O14 Ca3 C2A 159.35(19) 2_666 2_656 ?
O14 Ca3 C2A 92.2(2) . 2_656 ?
O14 Ca3 C4 95.8(2) . 2_666 ?
O14 Ca3 C4 23.7(2) 2_666 2_666 ?
O14 Ca3 C21 108.8(2) 2_666 2_656 ?
O14 Ca3 C21 171.5(2) . 2_656 ?
O14 Ca3 O2D 145.47(19) . 2_656 ?
O14 Ca3 O3 96.27(19) . 2_656 ?
O14 Ca3 O3 141.18(17) 2_666 2_656 ?
O14 Ca3 O13 75.3(2) . . ?
O14 Ca3 O14 72.3(3) . 2_666 ?
O14 Ca3 O17 85.0(2) . 2_656 ?
O14 Ca3 O18 162.1(3) . 2_656 ?
O14 Ca3 O19 76.2(2) . 2_666 ?
O16A Ca3 C2A 148.2(3) 2_666 2_656 ?
O16A Ca3 C4 28.2(3) 2_666 2_666 ?
O16A Ca3 C21 65.2(3) 2_666 2_656 ?
O16A Ca3 O2D 77.1(3) 2_666 2_656 ?
O16A Ca3 O3 140.4(3) 2_666 2_656 ?
O16A Ca3 O13 100.9(3) 2_666 . ?
O16A Ca3 O14 119.1(3) 2_666 . ?
O16A Ca3 O14 50.6(3) 2_666 2_666 ?
O16A Ca3 O17 144.3(3) 2_666 2_656 ?
O16A Ca3 O18 65.2(4) 2_666 2_656 ?
O16A Ca3 O19 81.3(4) 2_666 2_666 ?
O17 Ca3 C2A 23.23(19) 2_656 2_656 ?
O17 Ca3 C4 168.9(3) 2_656 2_666 ?
O17 Ca3 C21 94.9(3) 2_656 2_656 ?
O17 Ca3 O2D 98.0(2) 2_656 2_656 ?
O17 Ca3 O3 47.51(18) 2_656 2_656 ?
O17 Ca3 O13 111.2(2) 2_656 . ?
O17 Ca3 O14 155.9(2) 2_656 2_666 ?
O17 Ca3 O18 84.2(3) 2_656 2_656 ?
O17 Ca3 O19 79.6(2) 2_656 2_666 ?
O18 Ca3 C2A 83.3(3) 2_656 2_656 ?
O18 Ca3 C4 92.2(3) 2_656 2_666 ?
O18 Ca3 C21 25.1(2) 2_656 2_656 ?
O18 Ca3 O2D 50.64(17) 2_656 2_656 ?
O18 Ca3 O3 86.8(2) 2_656 2_656 ?
O18 Ca3 O14 115.5(3) 2_656 2_666 ?
O19 Ca3 C2A 102.8(2) 2_666 2_656 ?
O19 Ca3 C4 89.8(3) 2_666 2_666 ?
O19 Ca3 C21 112.21(19) 2_666 2_656 ?
O19 Ca3 O2D 138.30(17) 2_666 2_656 ?
O19 Ca3 O3 127.1(2) 2_666 2_656 ?
O19 Ca3 O14 87.0(2) 2_666 2_666 ?
O19 Ca3 O18 87.92(19) 2_666 2_656 ?
C27 Ca4 Ca1 58.89(16) . 2_656 ?
C27 Ca4 Ca3 98.1(2) . . ?
C27 Ca4 Na2 60.81(15) . . ?
Ca1 Ca4 Ca3 65.54(7) 2_656 . ?
Ca1 Ca4 Na2 119.58(10) 2_656 . ?
Na2 Ca4 Ca3 120.96(10) . . ?
O1A Ca4 C27 24.75(18) 2_656 . ?
O1A Ca4 Ca1 34.29(12) 2_656 2_656 ?
O1A Ca4 Ca3 85.5(2) 2_656 . ?
O1A Ca4 Na2 85.55(13) 2_656 . ?
O1A Ca4 O2D 70.81(19) 2_656 2_656 ?
O1A Ca4 O7 50.07(18) 2_656 . ?
O1A Ca4 O13 68.1(2) 2_656 . ?
O1B Ca4 C27 95.3(3) . . ?
O1B Ca4 Ca1 146.6(3) . 2_656 ?
O1B Ca4 Ca3 101.4(2) . . ?
O1B Ca4 Na2 38.95(19) . . ?
O1B Ca4 O1A 118.8(3) . 2_656 ?
O1B Ca4 O2D 143.0(3) . 2_656 ?
O1B Ca4 O7 72.0(2) . . ?
O1B Ca4 O13 81.9(3) . . ?
O1C Ca4 C27 100.1(5) . . ?
O1C Ca4 Ca1 79.5(4) . 2_656 ?
O1C Ca4 Ca3 123.3(4) . . ?
O1C Ca4 Na2 114.8(4) . . ?
O1C Ca4 O1A 89.5(5) . 2_656 ?
O1C Ca4 O1B 129.4(5) . . ?
O1C Ca4 O2D 83.6(4) . 2_656 ?
O1C Ca4 O7 107.0(5) . . ?
O1C Ca4 O13 148.4(5) . . ?
O2D Ca4 C27 94.3(2) 2_656 . ?
O2D Ca4 Ca1 37.52(12) 2_656 2_656 ?
O2D Ca4 Ca3 41.79(14) 2_656 . ?
O2D Ca4 Na2 150.3(2) 2_656 . ?
O2D Ca4 O7 119.0(2) 2_656 . ?
O2D Ca4 O13 68.6(2) 2_656 . ?
O7 Ca4 C27 25.38(19) . . ?
O7 Ca4 Ca1 84.27(16) . 2_656 ?
O7 Ca4 Ca3 111.9(2) . . ?
O7 Ca4 Na2 35.53(13) . . ?
O7 Ca4 O13 76.0(2) . . ?
O8 Ca4 C27 80.8(3) . . ?
O8 Ca4 Ca1 118.5(2) . 2_656 ?
O8 Ca4 Ca3 78.1(2) . . ?
O8 Ca4 Na2 46.28(17) . . ?
O8 Ca4 O1A 99.0(3) . 2_656 ?
O8 Ca4 O1B 29.6(3) . . ?
O8 Ca4 O1C 157.8(5) . . ?
O8 Ca4 O2D 118.6(3) . 2_656 ?
O8 Ca4 O7 65.0(2) . . ?
O8 Ca4 O13 52.6(2) . . ?
O13 Ca4 C27 68.8(2) . . ?
O13 Ca4 Ca1 69.47(16) . 2_656 ?
O13 Ca4 Ca3 37.03(12) . . ?
O13 Ca4 Na2 86.33(14) . . ?
C24 N1 C26 127.0(5) . . ?
C25 N1 C24 108.2(5) . . ?
C25 N1 C26 124.7(6) . . ?
C4AA N2 C15 124.7(5) . . ?
C25 N2 C4AA 109.5(5) . . ?
C25 N2 C15 125.7(5) . . ?
C2 N3 C3A 120.8(10) . . ?
C2 N3 C3B 118.1(12) . . ?
C3AA N3 C2 129.7(7) . . ?
C3AA N3 C3A 98.4(11) . . ?
C3AA N3 C3B 101.6(10) . . ?
C3B N3 C3A 73.6(13) . . ?
C3AA N4 C4A 104.2(9) . . ?
C3AA N4 C4B 98.5(10) . . ?
C3AA N4 C6 131.5(6) . . ?
C4A N4 C4B 72.5(19) . . ?
C6 N4 C4A 118.4(11) . . ?
C6 N4 C4B 114.9(10) . . ?
C1A N5 C16 125.6(5) . . ?
C1A N5 C17 108.8(5) . . ?
C17 N5 C16 125.6(5) . . ?
C1A N6 C18 108.7(5) . . ?
C1A N6 C20 123.8(5) . . ?
C18 N6 C20 127.5(5) . . ?
C31 N7 C33 125.2(5) . . ?
C32 N7 C31 107.7(5) . . ?
C32 N7 C33 127.1(5) . . ?
C30 N8 C29 126.4(6) . . ?
C32 N8 C29 123.9(6) . . ?
C32 N8 C30 109.6(5) . . ?
C44 N9 C43 125.0(4) . . ?
C46 N9 C43 125.6(4) . . ?
C46 N9 C44 108.7(5) . . ?
C45 N10 C47 128.4(5) . . ?
C46 N10 C45 108.1(5) . . ?
C46 N10 C47 123.5(5) . . ?
C50 N11 C49 124.0(6) . . ?
C52 N11 C49 128.9(6) . . ?
C52 N11 C50 106.9(6) . . ?
C51 N12 C53 125.7(7) . . ?
C52 N12 C51 107.6(6) . . ?
C52 N12 C53 125.8(7) . . ?
O1B Na2 Ca4 36.1(2) . . ?
O1B Na2 O8 24.5(2) . . ?
O2C Na2 Ca4 85.66(14) . . ?
O2C Na2 O1B 74.3(2) . . ?
O2C Na2 O8 55.24(18) . . ?
O2C Na2 O12 78.3(3) . . ?
O4 Na2 Ca4 84.3(5) . . ?
O4 Na2 O1B 81.3(4) . . ?
O4 Na2 O2C 150.4(4) . . ?
O4 Na2 O7 106.9(5) . . ?
O4 Na2 O8 104.5(4) . . ?
O4 Na2 O10 79.0(4) . . ?
O4 Na2 O11 106.0(5) . . ?
O4 Na2 O12 80.3(6) . . ?
O7 Na2 Ca4 40.70(15) . . ?
O7 Na2 O1B 74.2(2) . . ?
O7 Na2 O2C 82.5(2) . . ?
O7 Na2 O8 59.9(2) . . ?
O7 Na2 O10 78.5(3) . . ?
O7 Na2 O11 129.5(2) . . ?
O7 Na2 O12 149.3(3) . . ?
O8 Na2 Ca4 34.51(15) . . ?
O10 Na2 Ca4 106.9(2) . . ?
O10 Na2 O1B 139.8(3) . . ?
O10 Na2 O2C 130.6(2) . . ?
O10 Na2 O8 137.7(3) . . ?
O10 Na2 O12 132.1(3) . . ?
O11 Na2 Ca4 168.73(19) . . ?
O11 Na2 O1B 148.3(3) . . ?
O11 Na2 O2C 87.3(2) . . ?
O11 Na2 O8 141.6(2) . . ?
O11 Na2 O10 71.5(2) . . ?
O11 Na2 O12 73.5(3) . . ?
O12 Na2 Ca4 113.5(2) . . ?
O12 Na2 O1B 77.6(3) . . ?
O12 Na2 O8 89.4(3) . . ?
C27 O1A Ca1 156.8(6) 2_656 . ?
C27 O1A Ca4 95.2(5) 2_656 2_656 ?
Ca1 O1A Ca4 106.63(19) . 2_656 ?
Ca4 O1B Na2 105.0(3) . . ?
O8 O1B Ca4 68.7(5) . . ?
O8 O1B Na2 92.9(5) . . ?
Ca4 O1C H1CA 120.0 . . ?
Ca4 O1C H1CB 119.8 . . ?
H1CA O1C H1CB 97.1 . . ?
C48 O2C Na2 150.0(5) . . ?
C21 O2D Ca1 122.0(5) . . ?
C21 O2D Ca3 86.7(5) . 2_656 ?
C21 O2D Ca4 130.2(6) . 2_656 ?
Ca1 O2D Ca3 113.4(3) . 2_656 ?
Ca1 O2D Ca4 101.65(19) . 2_656 ?
Ca4 O2D Ca3 97.62(18) 2_656 2_656 ?
C2A O3 Ca1 133.2(5) . . ?
C2A O3 Ca3 82.3(5) . 2_656 ?
Ca1 O3 Ca3 107.4(3) . 2_656 ?
Na2 O4 H4C 123.9 . . ?
Na2 O4 H4D 123.4 . . ?
H4C O4 H4D 92.0 . . ?
C28 O5 Ca1 95.3(4) . . ?
C28 O6 Ca1 90.1(4) 2_656 2_656 ?
C28 O6 Ca1 155.2(4) 2_656 . ?
Ca1 O6 Ca1 113.67(19) . 2_656 ?
C27 O7 Ca4 90.7(4) . . ?
C27 O7 Na2 164.1(5) . . ?
Na2 O7 Ca4 103.8(2) . . ?
Ca4 O8 Na2 99.2(3) . . ?
O1B O8 Ca4 81.7(5) . . ?
O1B O8 Na2 62.6(5) . . ?
Na2 O10 H10A 125.1 . . ?
Na2 O10 H10B 125.5 . . ?
H10A O10 H10B 109.4 . . ?
Na2 O11 H11A 125.4 . . ?
Na2 O11 H11B 125.4 . . ?
H11A O11 H11B 109.1 . . ?
Na2 O12 H12A 125.3 . . ?
Na2 O12 H12B 125.6 . . ?
H12A O12 H12B 109.0 . . ?
Ca3 O13 Ca4 101.1(2) . . ?
C4 O14 Ca3 159.2(7) . . ?
C4 O14 Ca3 91.8(7) . 2_666 ?
Ca3 O14 Ca3 107.7(2) . 2_666 ?
C4 O16A Ca3 101.4(6) . 2_666 ?
C4 O16A O16B 53.6(9) . . ?
O16B O16A Ca3 100.3(9) . 2_666 ?
C4 O16B O16A 62.4(13) . . ?
C2A O17 Ca3 106.9(6) . 2_656 ?
C21 O18 Ca3 96.5(5) . 2_656 ?
C48 O19 Ca3 141.2(6) . 2_666 ?
H9A O9 H9B 109.5 . . ?
H24A O24 H24B 109.5 . . ?
H15C O15 H15D 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1B C2B C9 C10 1.9(7) . . . . ?
C1B C2B C9 C15 -179.1(4) . . . . ?
C1B C6 N4 C3AA 12.2(15) . . . . ?
C1B C6 N4 C4A 161(2) . . . . ?
C1B C6 N4 C4B -116.7(11) . . . . ?
C2 C2A O3 Ca1 66.0(12) . . . . ?
C2 C2A O3 Ca3 172.8(7) . . . 2_656 ?
C2 C2A O17 Ca3 -171.0(6) . . . 2_656 ?
C2A C2 N3 C3A -69.0(18) . . . . ?
C2A C2 N3 C3AA 66.6(16) . . . . ?
C2A C2 N3 C3B -155.8(12) . . . . ?
C2B C1B C6 N4 82.7(8) . . . . ?
C2B C1B C12 C11 2.8(7) . . . . ?
C2B C1B C12 C13 -174.6(5) . . . . ?
C2B C9 C10 C3 175.4(5) . . . . ?
C2B C9 C10 C11 -3.5(7) . . . . ?
C2B C9 C15 N2 -98.6(6) . . . . ?
C3 C10 C11 C12 -174.1(5) . . . . ?
C3 C10 C11 C16 7.0(7) . . . . ?
C3A C3B C4B C4A -0.4(12) . . . . ?
C3A C3B C4B N4 50.0(12) . . . . ?
C3A C3B N3 C2 116.6(13) . . . . ?
C3A C3B N3 C3AA -95.4(11) . . . . ?
C3A C4A C4B C3B 0.6(16) . . . . ?
C3A C4A C4B N4 -107.6(14) . . . . ?
C3A C4A N4 C3AA -14(3) . . . . ?
C3A C4A N4 C4B 80(3) . . . . ?
C3A C4A N4 C6 -170(2) . . . . ?
C3B C3A C4A C4B -0.4(13) . . . . ?
C3B C3A C4A N4 -55(3) . . . . ?
C3B C3A N3 C2 -113.3(14) . . . . ?
C3B C3A N3 C3AA 99.7(12) . . . . ?
C3B C4B N4 C3AA 22.5(11) . . . . ?
C3B C4B N4 C4A -79.8(12) . . . . ?
C3B C4B N4 C6 166.3(11) . . . . ?
C4 C53 N12 C51 -50.1(12) . . . . ?
C4 C53 N12 C52 117.9(10) . . . . ?
C4A C3A C3B C4B 0.5(16) . . . . ?
C4A C3A C3B N3 109.6(15) . . . . ?
C4A C3A N3 C2 168(2) . . . . ?
C4A C3A N3 C3AA 21(3) . . . . ?
C4A C3A N3 C3B -79(3) . . . . ?
C4A C4B N4 C3AA 102.3(10) . . . . ?
C4A C4B N4 C6 -113.8(11) . . . . ?
C4AA C24 N1 C25 -1.4(8) . . . . ?
C4AA C24 N1 C26 -178.0(7) . . . . ?
C4B C3B N3 C2 -167.5(12) . . . . ?
C4B C3B N3 C3A 75.9(13) . . . . ?
C4B C3B N3 C3AA -19.5(12) . . . . ?
C4B C4A N4 C3AA -94.6(12) . . . . ?
C4B C4A N4 C6 109.3(14) . . . . ?
C6 C1B C2B C9 177.7(5) . . . . ?
C6 C1B C2B C14 -5.0(7) . . . . ?
C6 C1B C12 C11 -176.4(5) . . . . ?
C6 C1B C12 C13 6.3(7) . . . . ?
C9 C10 C11 C12 4.8(7) . . . . ?
C9 C10 C11 C16 -174.1(5) . . . . ?
C9 C15 N2 C4AA -157.1(6) . . . . ?
C9 C15 N2 C25 23.9(8) . . . . ?
C10 C9 C15 N2 80.5(6) . . . . ?
C10 C11 C12 C1B -4.4(7) . . . . ?
C10 C11 C12 C13 172.9(5) . . . . ?
C10 C11 C16 N5 -101.7(6) . . . . ?
C11 C16 N5 C1A 11.6(8) . . . . ?
C11 C16 N5 C17 -170.0(6) . . . . ?
C12 C1B C2B C9 -1.5(7) . . . . ?
C12 C1B C2B C14 175.8(5) . . . . ?
C12 C1B C6 N4 -98.1(8) . . . . ?
C12 C11 C16 N5 79.4(6) . . . . ?
C14 C2B C9 C10 -175.4(5) . . . . ?
C14 C2B C9 C15 3.6(7) . . . . ?
C15 C9 C10 C3 -3.6(7) . . . . ?
C15 C9 C10 C11 177.5(4) . . . . ?
C16 C11 C12 C1B 174.4(5) . . . . ?
C16 C11 C12 C13 -8.2(7) . . . . ?
C17 C18 N6 C1A -0.9(8) . . . . ?
C17 C18 N6 C20 -177.4(6) . . . . ?
C18 C17 N5 C1A 0.6(7) . . . . ?
C18 C17 N5 C16 -178.0(6) . . . . ?
C20 C21 O2D Ca1 -80.2(9) . . . . ?
C20 C21 O2D Ca3 164.1(7) . . . 2_656 ?
C20 C21 O2D Ca4 67.0(8) . . . 2_656 ?
C20 C21 O18 Ca3 -162.7(7) . . . 2_656 ?
C21 C20 N6 C1A -66.4(8) . . . . ?
C21 C20 N6 C18 109.6(8) . . . . ?
C24 C4AA N2 C15 -179.0(6) . . . . ?
C24 C4AA N2 C25 0.1(8) . . . . ?
C26 C27 O7 Ca4 170.2(7) . . . . ?
C26 C27 O7 Na2 14(3) . . . . ?
C27 C26 N1 C24 -72.6(10) . . . . ?
C27 C26 N1 C25 111.3(8) . . . . ?
C28 C29 N8 C30 72.7(10) . . . . ?
C28 C29 N8 C32 -104.2(7) . . . . ?
C29 C28 O5 Ca1 -179.5(5) . . . . ?
C30 C31 N7 C32 -2.7(10) . . . . ?
C30 C31 N7 C33 175.3(7) . . . . ?
C31 C30 N8 C29 179.3(7) . . . . ?
C31 C30 N8 C32 -3.4(11) . . . . ?
C33 C34 C35 C36 172.9(5) . . . . ?
C33 C34 C35 C40 -6.8(8) . . . . ?
C33 C34 C39 C1 3.9(7) . . . . ?
C33 C34 C39 C38 -177.4(5) . . . . ?
C34 C33 N7 C31 145.9(7) . . . . ?
C34 C33 N7 C32 -36.5(8) . . . . ?
C34 C35 C36 C37 6.3(8) . . . . ?
C34 C35 C36 C43 -175.4(5) . . . . ?
C35 C34 C39 C1 -176.2(5) . . . . ?
C35 C34 C39 C38 2.4(8) . . . . ?
C35 C36 C37 C38 -0.9(8) . . . . ?
C35 C36 C37 C42 178.4(5) . . . . ?
C35 C36 C43 N9 -101.5(6) . . . . ?
C36 C37 C38 C39 -3.7(8) . . . . ?
C36 C37 C38 C49 174.3(5) . . . . ?
C36 C43 N9 C44 172.0(5) . . . . ?
C36 C43 N9 C46 -18.8(8) . . . . ?
C37 C36 C43 N9 76.8(6) . . . . ?
C37 C38 C39 C1 -178.4(5) . . . . ?
C37 C38 C39 C34 3.0(8) . . . . ?
C37 C38 C49 N11 -83.7(7) . . . . ?
C38 C49 N11 C50 145.6(8) . . . . ?
C38 C49 N11 C52 -29.4(11) . . . . ?
C39 C34 C35 C36 -7.0(8) . . . . ?
C39 C34 C35 C40 173.4(5) . . . . ?
C39 C38 C49 N11 94.3(7) . . . . ?
C40 C35 C36 C37 -174.1(5) . . . . ?
C40 C35 C36 C43 4.2(7) . . . . ?
C42 C37 C38 C39 176.9(5) . . . . ?
C42 C37 C38 C49 -5.1(8) . . . . ?
C43 C36 C37 C38 -179.2(5) . . . . ?
C43 C36 C37 C42 0.1(8) . . . . ?
C44 C45 N10 C46 0.7(7) . . . . ?
C44 C45 N10 C47 -177.7(6) . . . . ?
C45 C44 N9 C43 170.7(5) . . . . ?
C45 C44 N9 C46 0.0(7) . . . . ?
C47 C48 O2C Na2 156.3(7) . . . . ?
C47 C48 O19 Ca3 -2.1(12) . . . 2_666 ?
C48 C47 N10 C45 -70.8(9) . . . . ?
C48 C47 N10 C46 110.9(7) . . . . ?
C49 C38 C39 C1 3.7(8) . . . . ?
C49 C38 C39 C34 -175.0(5) . . . . ?
C50 C51 N12 C52 8.2(12) . . . . ?
C50 C51 N12 C53 178.1(9) . . . . ?
C51 C50 N11 C49 -178.3(9) . . . . ?
C51 C50 N11 C52 -2.4(12) . . . . ?
C53 C4 O14 Ca3 171.3(10) . . . 2_666 ?
C53 C4 O14 Ca3 11(3) . . . . ?
C53 C4 O16A Ca3 -174.0(9) . . . 2_666 ?
C53 C4 O16A O16B 91.6(15) . . . . ?
C53 C4 O16B O16A -119.3(9) . . . . ?
Ca3 C2A O3 Ca1 -106.8(8) 2_656 . . . ?
Ca3 C4 O14 Ca3 -160(2) 2_666 . . . ?
Ca3 C4 O16A O16B -94.4(11) 2_666 . . . ?
Ca3 C4 O16B O16A 52.0(7) 2_666 . . . ?
Ca3 C21 O2D Ca1 115.6(5) 2_656 . . . ?
Ca3 C21 O2D Ca4 -97.2(5) 2_656 . . 2_656 ?
Ca3 O16A O16B C4 -96.7(9) 2_666 . . . ?
Ca4 C27 O7 Na2 -156(2) . . . . ?
Ca4 O1B O8 Na2 -104.9(3) . . . . ?
N1 C25 N2 C4AA -1.0(7) . . . . ?
N1 C25 N2 C15 178.1(5) . . . . ?
N1 C26 C27 O1A -177.1(7) . . . 2_656 ?
N1 C26 C27 O7 6.5(12) . . . . ?
N2 C4AA C24 N1 0.7(8) . . . . ?
N2 C25 N1 C24 1.4(7) . . . . ?
N2 C25 N1 C26 178.2(6) . . . . ?
N3 C2 C2A Ca3 -5(3) . . . 2_656 ?
N3 C2 C2A O3 -155.0(8) . . . . ?
N3 C2 C2A O17 25.0(11) . . . . ?
N3 C3A C3B C4B -109.0(13) . . . . ?
N3 C3A C4A C4B 51(2) . . . . ?
N3 C3A C4A N4 -4(3) . . . . ?
N3 C3AA N4 C4A 33(2) . . . . ?
N3 C3AA N4 C4B -40.9(14) . . . . ?
N3 C3AA N4 C6 -175.3(11) . . . . ?
N3 C3B C4B C4A -52.2(13) . . . . ?
N3 C3B C4B N4 -1.8(12) . . . . ?
N4 C3AA N3 C2 -176.5(12) . . . . ?
N4 C3AA N3 C3A -33.9(16) . . . . ?
N4 C3AA N3 C3B 40.9(15) . . . . ?
N4 C4A C4B C3B 108.1(13) . . . . ?
N5 C1A N6 C18 1.3(7) . . . . ?
N5 C1A N6 C20 178.0(5) . . . . ?
N5 C17 C18 N6 0.2(8) . . . . ?
N6 C1A N5 C16 177.4(5) . . . . ?
N6 C1A N5 C17 -1.2(7) . . . . ?
N6 C20 C21 Ca3 -90(2) . . . 2_656 ?
N6 C20 C21 O2D 171.1(7) . . . . ?
N6 C20 C21 O18 -7.8(11) . . . . ?
N7 C32 N8 C29 179.1(5) . . . . ?
N7 C32 N8 C30 1.7(8) . . . . ?
N7 C33 C34 C35 111.3(6) . . . . ?
N7 C33 C34 C39 -68.8(6) . . . . ?
N8 C30 C31 N7 3.6(11) . . . . ?
N8 C32 N7 C31 0.6(7) . . . . ?
N8 C32 N7 C33 -177.4(5) . . . . ?
N9 C44 C45 N10 -0.5(7) . . . . ?
N9 C46 N10 C45 -0.7(7) . . . . ?
N9 C46 N10 C47 177.8(6) . . . . ?
N10 C46 N9 C43 -170.2(5) . . . . ?
N10 C46 N9 C44 0.4(7) . . . . ?
N10 C47 C48 O2C 12.5(9) . . . . ?
N10 C47 C48 O19 -170.0(6) . . . . ?
N11 C50 C51 N12 -3.5(13) . . . . ?
N11 C52 N12 C51 -10.1(10) . . . . ?
N11 C52 N12 C53 -179.9(8) . . . . ?
N12 C52 N11 C49 -176.4(7) . . . . ?
N12 C52 N11 C50 7.9(10) . . . . ?
Na2 O1B O8 Ca4 104.9(3) . . . . ?
O1A C27 O7 Ca4 -5.9(10) 2_656 . . . ?
O1A C27 O7 Na2 -162.2(17) 2_656 . . . ?
O2C C48 O19 Ca3 175.3(6) . . . 2_666 ?
O2D C21 O18 Ca3 18.5(10) . . . 2_656 ?
O3 C2A O17 Ca3 8.9(10) . . . 2_656 ?
O5 C28 C29 N8 -18.1(9) . . . . ?
O6 C28 C29 N8 164.5(6) 2_656 . . . ?
O6 C28 O5 Ca1 -2.3(8) 2_656 . . . ?
O14 C4 C53 N12 -170.3(10) . . . . ?
O14 C4 O16A Ca3 -24.4(10) . . . 2_666 ?
O14 C4 O16A O16B -118.8(12) . . . . ?
O14 C4 O16B O16A 98.3(17) . . . . ?
O16A C4 C53 N12 -23.2(15) . . . . ?
O16A C4 O14 Ca3 -139.7(19) . . . . ?
O16A C4 O14 Ca3 20.7(9) . . . 2_666 ?
O16B C4 C53 N12 45.2(14) . . . . ?
O16B C4 O14 Ca3 -51(2) . . . 2_666 ?
O16B C4 O14 Ca3 148(2) . . . . ?
O16B C4 O16A Ca3 94.4(11) . . . 2_666 ?
O17 C2A O3 Ca1 -113.9(9) . . . . ?
O17 C2A O3 Ca3 -7.1(8) . . . 2_656 ?
O18 C21 O2D Ca1 98.6(9) . . . . ?
O18 C21 O2D Ca3 -17.0(9) . . . 2_656 ?
O18 C21 O2D Ca4 -114.2(11) . . . 2_656 ?
O19 C48 O2C Na2 -21.0(14) . . . . ?


_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.929 Note  
RESPONSE: Crystals were weakly diffracting and this is reflected in the 
low fraction of measured reflections. Although recrystallization and 
data collection for different crystals was attempted repeatedly, but 
this structure represents the best of the all.
;

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_6
_database_code_depnum_ccdc_archive 'CCDC 1024410'
_audit_update_record             
;
2015-03-02 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_audit_creation_date             2015-03-02
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        6
_chemical_formula_moiety         'C78 H88 Ca2.5 N12 O20, 6(Br)'
_chemical_formula_sum            'C78 H88 Br6 Ca2.50 N12 O20'
_chemical_formula_weight         2093.26
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.3416(7)
_cell_length_b                   20.7798(8)
_cell_length_c                   21.1629(8)
_cell_angle_alpha                89.717(3)
_cell_angle_beta                 74.471(4)
_cell_angle_gamma                75.245(4)
_cell_volume                     5862.7(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22056
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      70.85
_cell_measurement_theta_min      3.20
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.898
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   
'Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22056
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.853
_diffrn_reflns_theta_min         3.198
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         22056
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15092
_reflns_number_total             22056
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_refine_diff_density_max         3.204
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         22056
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0995
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2967
_refine_ls_wR_factor_ref         0.3199
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H7A-H28D
 2.2 with sigma of 0.02
3. Others
 Fixed Sof: O28(0.5) H28C(0.5) H28D(0.5) O1A(0.5) H1AA(0.5) H1AB(0.5) Ca1B(0.5)
4.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10C,H10D), O11(H11A,H11B),
 O12(H12A,H12B), O13(H13A,H13B), O28(H28C,H28D), O1A(H1AA,H1AB)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C20(H20A,H20B), C28(H28A,H28B), C30(H30A,H30B),
 C38(H38A,H38B), C41(H41A,H41B), C49(H49A,H49B), C59(H59A,H59B), C67(H67A,H67B),
  C69(H69A,H69B), C77(H77A,H77B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C22(H22), C23(H23), C24(H24),
 C25(H25), C27(H27), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C61(H61), C62(H62), C63(H63),
 C64(H64), C66(H66), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3894(5) 0.8695(3) -0.3369(3) 0.0405(14) Uani 1 1 d . . . . .
C2 C 0.4763(5) 0.8632(3) -0.3972(3) 0.0384(13) Uani 1 1 d . . . . .
H2A H 0.5227 0.8877 -0.3881 0.046 Uiso 1 1 calc R . . . .
H2B H 0.5135 0.8157 -0.4076 0.046 Uiso 1 1 calc R . . . .
C3 C 0.4007(5) 0.9572(3) -0.4615(3) 0.0387(13) Uani 1 1 d . . . . .
C4 C 0.3907(5) 1.0144(3) -0.4242(3) 0.0426(14) Uani 1 1 d . . . . .
H4 H 0.4096 1.0121 -0.3844 0.051 Uiso 1 1 calc R . . . .
C5 C 0.3523(6) 1.0747(3) -0.4471(3) 0.0470(16) Uani 1 1 d . . . . .
H5 H 0.3455 1.1151 -0.4233 0.056 Uiso 1 1 calc R . . . .
C6 C 0.3222(6) 1.0772(4) -0.5074(3) 0.0528(18) Uani 1 1 d . . . . .
H6 H 0.2940 1.1192 -0.5218 0.063 Uiso 1 1 calc R . . . .
C7 C 0.3336(5) 1.0197(3) -0.5442(3) 0.0431(14) Uani 1 1 d . . . . .
H7 H 0.3125 1.0210 -0.5832 0.052 Uiso 1 1 calc R . . . .
C8 C 0.3775(5) 0.9597(3) -0.5214(3) 0.0377(13) Uani 1 1 d . . . . .
C9 C 0.4414(5) 0.8545(3) -0.5051(3) 0.0370(13) Uani 1 1 d . . . . .
H9 H 0.4634 0.8073 -0.5113 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3898(5) 0.8739(3) -0.6106(3) 0.0439(15) Uani 1 1 d . . . . .
H10A H 0.4038 0.9070 -0.6432 0.053 Uiso 1 1 calc R . . . .
H10B H 0.3188 0.8735 -0.6033 0.053 Uiso 1 1 calc R . . . .
C11 C 0.4562(5) 0.8061(3) -0.6381(3) 0.0381(13) Uani 1 1 d . . . . .
C12 C 0.5473(5) 0.7995(3) -0.6845(3) 0.0340(12) Uani 1 1 d . . . . .
C13 C 0.6047(4) 0.7356(3) -0.7143(3) 0.0312(11) Uani 1 1 d . . . . .
C14 C 0.5732(5) 0.6777(3) -0.6926(3) 0.0364(12) Uani 1 1 d . . . . .
C15 C 0.4840(5) 0.6836(3) -0.6454(3) 0.0326(12) Uani 1 1 d . . . . .
C16 C 0.4207(4) 0.7483(3) -0.6181(3) 0.0370(13) Uani 1 1 d . . . . .
C17 C 0.5862(5) 0.8605(3) -0.7018(3) 0.0404(13) Uani 1 1 d . . . . .
H17A H 0.5603 0.8819 -0.7373 0.061 Uiso 1 1 calc GR . . . .
H17B H 0.6596 0.8470 -0.7163 0.061 Uiso 1 1 calc GR . . . .
H17C H 0.5637 0.8919 -0.6631 0.061 Uiso 1 1 calc GR . . . .
C18 C 0.3220(5) 0.7536(4) -0.5671(3) 0.0493(16) Uani 1 1 d . . . . .
H18A H 0.2827 0.8003 -0.5596 0.074 Uiso 1 1 calc GR . . . .
H18B H 0.3347 0.7372 -0.5259 0.074 Uiso 1 1 calc GR . . . .
H18C H 0.2846 0.7267 -0.5829 0.074 Uiso 1 1 calc GR . . . .
C19 C 0.6411(5) 0.6095(3) -0.7207(3) 0.0412(14) Uani 1 1 d . . . . .
H19A H 0.6235 0.5958 -0.7593 0.062 Uiso 1 1 calc GR . . . .
H19B H 0.6326 0.5770 -0.6874 0.062 Uiso 1 1 calc GR . . . .
H19C H 0.7111 0.6117 -0.7336 0.062 Uiso 1 1 calc GR . . . .
C20 C 0.4492(5) 0.6231(3) -0.6223(3) 0.0421(14) Uani 1 1 d . . . . .
H20A H 0.3794 0.6295 -0.6246 0.050 Uiso 1 1 calc R . . . .
H20B H 0.4918 0.5839 -0.6521 0.050 Uiso 1 1 calc R . . . .
C21 C 0.3914(6) 0.5774(3) -0.5110(3) 0.0459(15) Uani 1 1 d . . . . .
C22 C 0.3145(6) 0.5511(4) -0.5165(4) 0.0500(16) Uani 1 1 d . . . . .
H22 H 0.2950 0.5525 -0.5561 0.060 Uiso 1 1 calc R . . . .
C23 C 0.2672(6) 0.5227(4) -0.4625(4) 0.061(2) Uani 1 1 d . . . . .
H23 H 0.2160 0.5025 -0.4656 0.073 Uiso 1 1 calc R . . . .
C24 C 0.2933(8) 0.5229(5) -0.4012(4) 0.073(2) Uani 1 1 d . . . . .
H24 H 0.2555 0.5061 -0.3639 0.087 Uiso 1 1 calc R . . . .
C25 C 0.3736(7) 0.5474(4) -0.3961(4) 0.059(2) Uani 1 1 d . . . . .
H25 H 0.3933 0.5464 -0.3566 0.071 Uiso 1 1 calc R . . . .
C26 C 0.4236(6) 0.5737(3) -0.4532(3) 0.0467(15) Uani 1 1 d . . . . .
C27 C 0.5197(7) 0.6238(4) -0.5276(3) 0.0560(19) Uani 1 1 d . . . . .
H27 H 0.5711 0.6445 -0.5479 0.067 Uiso 1 1 calc R . . . .
C28 C 0.5516(7) 0.6172(4) -0.4171(4) 0.060(2) Uani 1 1 d . . . . .
H28A H 0.6189 0.6215 -0.4413 0.072 Uiso 1 1 calc R . . . .
H28B H 0.5616 0.5783 -0.3901 0.072 Uiso 1 1 calc R . . . .
C29 C 0.4971(7) 0.6804(4) -0.3701(4) 0.0536(18) Uani 1 1 d . . . . .
C30 C 0.7002(4) 0.7298(3) -0.7693(3) 0.0345(12) Uani 1 1 d . . . . .
H30A H 0.7052 0.6957 -0.8033 0.041 Uiso 1 1 calc R . . . .
H30B H 0.6965 0.7730 -0.7898 0.041 Uiso 1 1 calc R . . . .
C31 C 0.8906(5) 0.7007(3) -0.7861(3) 0.0384(13) Uani 1 1 d . . . . .
C32 C 0.9290(5) 0.7064(4) -0.8515(3) 0.0455(15) Uani 1 1 d . . . . .
H32 H 0.8863 0.7191 -0.8793 0.055 Uiso 1 1 calc R . . . .
C33 C 1.0313(6) 0.6932(4) -0.8758(4) 0.0532(17) Uani 1 1 d . . . . .
H33 H 1.0604 0.6974 -0.9211 0.064 Uiso 1 1 calc R . . . .
C34 C 1.0926(6) 0.6738(4) -0.8342(4) 0.063(2) Uani 1 1 d . . . . .
H34 H 1.1631 0.6660 -0.8519 0.076 Uiso 1 1 calc R . . . .
C35 C 1.0555(6) 0.6654(4) -0.7687(4) 0.0544(17) Uani 1 1 d . . . . .
H35 H 1.0990 0.6508 -0.7416 0.065 Uiso 1 1 calc R . . . .
C36 C 0.9529(5) 0.6790(3) -0.7436(3) 0.0456(15) Uani 1 1 d . . . . .
C37 C 0.7942(5) 0.6976(3) -0.6842(3) 0.0419(14) Uani 1 1 d . . . . .
H37 H 0.7374 0.7001 -0.6479 0.050 Uiso 1 1 calc R . . . .
C38 C 0.9180(6) 0.6548(4) -0.6227(3) 0.0513(17) Uani 1 1 d . . . . .
H38A H 0.9847 0.6610 -0.6242 0.062 Uiso 1 1 calc R . . . .
H38B H 0.8688 0.6818 -0.5838 0.062 Uiso 1 1 calc R . . . .
C39 C 0.9207(7) 0.5845(5) -0.6144(4) 0.063(2) Uani 1 1 d . . . . .
C40 C 0.3966(5) 0.8443(3) -0.1165(3) 0.0416(14) Uani 1 1 d . . . . .
C41 C 0.3570(5) 0.8963(3) -0.0597(3) 0.0450(15) Uani 1 1 d . . . . .
H41A H 0.3375 0.9407 -0.0769 0.054 Uiso 1 1 calc R . . . .
H41B H 0.2957 0.8880 -0.0299 0.054 Uiso 1 1 calc R . . . .
C42 C 0.5173(5) 0.9169(3) -0.0464(3) 0.0392(13) Uani 1 1 d . . . . .
C43 C 0.5590(6) 0.9393(3) -0.1055(3) 0.0506(17) Uani 1 1 d . . . . .
H43 H 0.5270 0.9449 -0.1398 0.061 Uiso 1 1 calc R . . . .
C44 C 0.6514(6) 0.9534(4) -0.1125(4) 0.0562(18) Uani 1 1 d . . . . .
H44 H 0.6842 0.9674 -0.1534 0.067 Uiso 1 1 calc R . . . .
C45 C 0.6967(6) 0.9477(4) -0.0614(4) 0.0561(18) Uani 1 1 d . . . . .
H45 H 0.7591 0.9583 -0.0681 0.067 Uiso 1 1 calc R . . . .
C46 C 0.6532(5) 0.9269(4) -0.0015(3) 0.0472(15) Uani 1 1 d . . . . .
H46 H 0.6841 0.9231 0.0333 0.057 Uiso 1 1 calc R . . . .
C47 C 0.5634(5) 0.9120(3) 0.0058(3) 0.0385(13) Uani 1 1 d . . . . .
C48 C 0.4220(5) 0.8817(3) 0.0392(3) 0.0388(13) Uani 1 1 d . . . . .
H48 H 0.3674 0.8677 0.0666 0.047 Uiso 1 1 calc R . . . .
C49 C 0.5180(5) 0.8772(3) 0.1236(3) 0.0363(12) Uani 1 1 d . . . . .
H49A H 0.4794 0.9171 0.1536 0.044 Uiso 1 1 calc R . . . .
H49B H 0.5900 0.8707 0.1202 0.044 Uiso 1 1 calc R . . . .
C50 C 0.4851(5) 0.8169(3) 0.1507(3) 0.0345(12) Uani 1 1 d . . . . .
C51 C 0.3945(4) 0.8241(3) 0.1990(2) 0.0307(11) Uani 1 1 d . . . . .
C52 C 0.3645(4) 0.7672(3) 0.2201(3) 0.0335(12) Uani 1 1 d . . . . .
C53 C 0.4203(5) 0.7033(3) 0.1920(3) 0.0352(12) Uani 1 1 d . . . . .
C54 C 0.5151(4) 0.6967(3) 0.1466(2) 0.0306(11) Uani 1 1 d . . . . .
C55 C 0.5479(5) 0.7527(3) 0.1257(3) 0.0318(11) Uani 1 1 d . . . . .
C56 C 0.6472(5) 0.7470(4) 0.0760(3) 0.0461(15) Uani 1 1 d . . . . .
H56A H 0.6360 0.7609 0.0337 0.069 Uiso 1 1 calc GR . . . .
H56B H 0.6878 0.7006 0.0707 0.069 Uiso 1 1 calc GR . . . .
H56C H 0.6825 0.7758 0.0912 0.069 Uiso 1 1 calc GR . . . .
C57 C 0.3307(5) 0.8925(3) 0.2267(3) 0.0361(12) Uani 1 1 d . . . . .
H57A H 0.3705 0.9165 0.2437 0.054 Uiso 1 1 calc GR . . . .
H57B H 0.2730 0.8886 0.2623 0.054 Uiso 1 1 calc GR . . . .
H57C H 0.3069 0.9172 0.1919 0.054 Uiso 1 1 calc GR . . . .
C58 C 0.3792(5) 0.6428(3) 0.2080(3) 0.0402(13) Uani 1 1 d . . . . .
H58A H 0.4008 0.6218 0.2450 0.060 Uiso 1 1 calc GR . . . .
H58B H 0.4044 0.6108 0.1695 0.060 Uiso 1 1 calc GR . . . .
H58C H 0.3057 0.6569 0.2197 0.060 Uiso 1 1 calc GR . . . .
C59 C 0.5794(5) 0.6274(3) 0.1214(3) 0.0384(13) Uani 1 1 d . . . . .
H59A H 0.6497 0.6251 0.1201 0.046 Uiso 1 1 calc R . . . .
H59B H 0.5570 0.5951 0.1526 0.046 Uiso 1 1 calc R . . . .
C60 C 0.6110(4) 0.5413(3) 0.0270(3) 0.0333(11) Uani 1 1 d . . . . .
C61 C 0.6513(5) 0.4828(3) 0.0513(3) 0.0413(13) Uani 1 1 d . . . . .
H61 H 0.6636 0.4815 0.0933 0.050 Uiso 1 1 calc R . . . .
C62 C 0.6734(6) 0.4254(3) 0.0109(3) 0.0457(15) Uani 1 1 d . . . . .
H62 H 0.6983 0.3832 0.0264 0.055 Uiso 1 1 calc R . . . .
C63 C 0.6595(5) 0.4283(3) -0.0526(3) 0.0423(14) Uani 1 1 d . . . . .
H63 H 0.6774 0.3881 -0.0795 0.051 Uiso 1 1 calc R . . . .
C64 C 0.6208(6) 0.4875(3) -0.0769(3) 0.0434(14) Uani 1 1 d . . . . .
H64 H 0.6111 0.4892 -0.1196 0.052 Uiso 1 1 calc R . . . .
C65 C 0.5967(5) 0.5444(3) -0.0362(3) 0.0360(12) Uani 1 1 d . . . . .
C66 C 0.5434(5) 0.6470(3) 0.0109(3) 0.0380(13) Uani 1 1 d . . . . .
H66 H 0.5162 0.6940 0.0178 0.046 Uiso 1 1 calc R . . . .
C67 C 0.5323(5) 0.6390(3) -0.1030(3) 0.0379(13) Uani 1 1 d . . . . .
H67A H 0.4891 0.6852 -0.0924 0.046 Uiso 1 1 calc R . . . .
H67B H 0.4945 0.6121 -0.1193 0.046 Uiso 1 1 calc R . . . .
C68 C 0.6238(6) 0.6394(3) -0.1555(3) 0.0464(15) Uani 1 1 d . . . . .
C69 C 0.2668(5) 0.7740(3) 0.2733(3) 0.0366(12) Uani 1 1 d . . . . .
H69A H 0.2666 0.7304 0.2923 0.044 Uiso 1 1 calc R . . . .
H69B H 0.2624 0.8063 0.3089 0.044 Uiso 1 1 calc R . . . .
C70 C 0.0762(5) 0.8128(4) 0.2863(3) 0.0462(15) Uani 1 1 d . . . . .
C71 C 0.0348(7) 0.8073(4) 0.3498(4) 0.059(2) Uani 1 1 d . . . . .
H71 H 0.0745 0.7924 0.3791 0.071 Uiso 1 1 calc R . . . .
C72 C -0.0697(7) 0.8245(5) 0.3709(4) 0.077(3) Uani 1 1 d . . . . .
H72 H -0.1026 0.8197 0.4154 0.093 Uiso 1 1 calc R . . . .
C73 C -0.1269(6) 0.8487(5) 0.3272(4) 0.075(3) Uani 1 1 d . . . . .
H73 H -0.1979 0.8612 0.3434 0.090 Uiso 1 1 calc R . . . .
C74 C -0.0834(6) 0.8553(5) 0.2606(4) 0.063(2) Uani 1 1 d . . . . .
H74 H -0.1220 0.8721 0.2311 0.076 Uiso 1 1 calc R . . . .
C75 C 0.0204(6) 0.8354(4) 0.2411(4) 0.0534(17) Uani 1 1 d . . . . .
C76 C 0.1818(5) 0.8093(3) 0.1852(3) 0.0424(14) Uani 1 1 d . . . . .
H76 H 0.2413 0.8029 0.1500 0.051 Uiso 1 1 calc R . . . .
C77 C 0.0670(6) 0.8559(4) 0.1189(4) 0.0557(18) Uani 1 1 d . . . . .
H77A H -0.0063 0.8671 0.1247 0.067 Uiso 1 1 calc R . . . .
H77B H 0.0994 0.8199 0.0834 0.067 Uiso 1 1 calc R . . . .
C78 C 0.1059(7) 0.9183(4) 0.0987(4) 0.061(2) Uani 1 1 d . . . . .
Ca0A Ca 0.49599(9) 0.75803(6) -0.23705(6) 0.0376(3) Uani 1 1 d . . . . .
Ca2 Ca 0.23610(10) 0.89753(7) -0.21438(6) 0.0435(3) Uani 1 1 d . . . . .
N1 N 0.4428(4) 0.8898(2) -0.4538(2) 0.0355(10) Uani 1 1 d . . . . .
N2 N 0.4046(4) 0.8951(2) -0.5474(2) 0.0361(10) Uani 1 1 d . . . . .
N3 N 0.5016(5) 0.6032(3) -0.4649(3) 0.0526(15) Uani 1 1 d . . . . .
N4 N 0.4531(5) 0.6099(3) -0.5554(3) 0.0438(12) Uani 1 1 d . . . . .
N5 N 0.4284(4) 0.8979(3) -0.0216(2) 0.0401(11) Uani 1 1 d . . . . .
N6 N 0.5007(4) 0.8872(2) 0.0575(2) 0.0364(11) Uani 1 1 d . . . . .
N7 N 0.5542(4) 0.6117(2) -0.0428(2) 0.0358(11) Uani 1 1 d . . . . .
N8 N 0.5761(4) 0.6072(2) 0.0550(2) 0.0328(10) Uani 1 1 d . . . . .
N9 N 0.8910(4) 0.6798(3) -0.6824(3) 0.0466(13) Uani 1 1 d . . . . .
N10 N 0.7920(4) 0.7114(3) -0.7461(2) 0.0374(11) Uani 1 1 d . . . . .
N11 N 0.0881(5) 0.8325(3) 0.1795(3) 0.0481(13) Uani 1 1 d . . . . .
N12 N 0.1791(4) 0.7965(3) 0.2480(2) 0.0378(11) Uani 1 1 d . . . . .
O2 O 0.4123(4) 0.8441(2) -0.2868(2) 0.0436(10) Uani 1 1 d . . . . .
O1 O 0.3374(4) 0.8399(2) -0.1493(2) 0.0515(12) Uani 1 1 d . . . . .
O3 O 0.4877(4) 0.8101(2) -0.1308(2) 0.0487(11) Uani 1 1 d . . . . .
O4 O 0.3040(4) 0.8983(3) -0.3380(2) 0.0546(13) Uani 1 1 d . . . . .
O5 O 0.6124(4) 0.6711(2) -0.2059(2) 0.0553(13) Uani 1 1 d . . . . .
O2A O 0.5479(4) 0.6920(3) -0.3341(2) 0.0569(13) Uani 1 1 d . . . . .
O7 O 0.6370(4) 0.8050(2) -0.2825(2) 0.0506(11) Uani 1 1 d . . . . .
H7A H 0.7013 0.7813 -0.3000 0.076 Uiso 1 1 d DGR . . . .
H7B H 0.6334 0.8490 -0.2848 0.076 Uiso 1 1 d GR . . . .
O8 O 0.3793(4) 0.6937(2) -0.2009(3) 0.0567(13) Uani 1 1 d . . . . .
H8A H 0.3511 0.6852 -0.1564 0.085 Uiso 1 1 d GR . . . .
H8B H 0.3528 0.6716 -0.2287 0.085 Uiso 1 1 d GR . . . .
O9 O 0.3325(4) 0.9789(3) -0.2203(3) 0.083(2) Uani 1 1 d . . . . .
H9A H 0.3054 1.0286 -0.2007 0.125 Uiso 1 1 d GR . . . .
H9B H 0.4096 0.9706 -0.2425 0.125 Uiso 1 1 d GR . . . .
O10 O 0.2335(5) 0.7886(3) -0.2601(3) 0.0685(15) Uani 1 1 d . . . . .
H10C H 0.2263 0.7541 -0.2273 0.103 Uiso 1 1 d GR . . . .
H10D H 0.2951 0.7661 -0.2950 0.103 Uiso 1 1 d GR . . . .
O11 O 0.0969(5) 0.9537(4) -0.2524(3) 0.099(3) Uani 1 1 d . . . . .
H11A H 0.0226 0.9553 -0.2308 0.148 Uiso 1 1 d GR . . . .
H11B H 0.0989 0.9815 -0.2932 0.148 Uiso 1 1 d GR . . . .
O12 O 0.1174(4) 0.8492(3) -0.1359(3) 0.0601(13) Uani 1 1 d . . . . .
H12A H 0.0431 0.8695 -0.1190 0.090 Uiso 1 1 d GR . . . .
H12B H 0.1343 0.8058 -0.1148 0.090 Uiso 1 1 d GR . . . .
O13 O 0.1566(5) 0.9835(3) -0.1221(3) 0.0723(17) Uani 1 1 d . . . . .
H13A H 0.1656 0.9683 -0.0798 0.108 Uiso 1 1 d GR . . . .
H13B H 0.0842 1.0005 -0.1139 0.108 Uiso 1 1 d GR . . . .
O14 O 0.7074(4) 0.6091(3) -0.1491(3) 0.0629(15) Uani 1 1 d . . . . .
O6 O 0.4104(6) 0.7105(3) -0.3726(4) 0.084(2) Uani 1 1 d . . . . .
O16 O 0.9171(8) 0.5503(4) -0.6622(4) 0.108(3) Uani 1 1 d . . . . .
O17 O 0.9382(5) 0.5599(4) -0.5639(3) 0.0747(18) Uani 1 1 d . . . . .
O18 O 0.0629(7) 0.9498(4) 0.0608(5) 0.102(3) Uani 1 1 d . . . A -1
O19 O 0.1702(4) 0.9295(3) 0.1197(4) 0.0698(16) Uani 1 1 d . . . . .
O28 O 0.7896(9) 0.7213(6) -0.2322(7) 0.066(3) Uani 0.5 1 d . . P . .
H28C H 0.7443 0.7476 -0.1941 0.099 Uiso 0.5 1 d GR . P . .
H28D H 0.8282 0.7483 -0.2580 0.099 Uiso 0.5 1 d DGR . P . .
Br1 Br 0.56894(6) 0.96722(4) -0.27981(4) 0.0513(2) Uani 1 1 d . . . . .
Br2 Br 0.46640(7) 0.53085(4) -0.23667(4) 0.0538(2) Uani 1 1 d . . . B 1
Br3 Br 0.31299(7) 0.75359(4) 0.02886(4) 0.0592(2) Uani 1 1 d . . . . .
Br5 Br 0.22748(7) 1.12114(5) -0.13740(5) 0.0655(3) Uani 1 1 d . . . . .
Br6 Br 0.80731(9) 0.37382(7) -0.35941(6) 0.0858(3) Uani 1 1 d . . . . .
Br4 Br 0.66303(7) 0.73682(5) -0.52500(4) 0.0624(2) Uani 1 1 d . . . . .
O1A O 0.7546(7) 0.6381(5) -0.3547(5) 0.050(2) Uani 0.5 1 d . . P . .
H1AA H 0.8058 0.6148 -0.4062 0.076 Uiso 0.5 1 d GR . P . .
H1AB H 0.7411 0.6940 -0.3690 0.076 Uiso 0.5 1 d GR . P . .
Ca1B Ca 0.8038(2) 0.60420(14) -0.25912(14) 0.0501(7) Uani 0.5 1 d . . P . .


_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
C1 C2 1.505(9) . ?
C1 Ca2 2.865(7) . ?
C1 O2 1.268(7) . ?
C1 O4 1.224(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N1 1.462(7) . ?
C3 C4 1.385(9) . ?
C3 C8 1.391(8) . ?
C3 N1 1.406(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.376(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.448(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(10) . ?
C7 H7 0.9500 . ?
C7 C8 1.393(9) . ?
C8 N2 1.374(8) . ?
C9 H9 0.9500 . ?
C9 N1 1.321(8) . ?
C9 N2 1.344(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.503(9) . ?
C10 N2 1.494(8) . ?
C11 C12 1.383(9) . ?
C11 C16 1.440(9) . ?
C12 C13 1.418(8) . ?
C12 C17 1.515(8) . ?
C13 C14 1.423(8) . ?
C13 C30 1.520(8) . ?
C14 C15 1.374(9) . ?
C14 C19 1.518(9) . ?
C15 C16 1.439(9) . ?
C15 C20 1.501(8) . ?
C16 C18 1.510(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 N4 1.453(7) . ?
C21 C22 1.380(10) . ?
C21 C26 1.414(9) . ?
C21 N4 1.407(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.442(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.401(13) . ?
C25 H25 0.9500 . ?
C25 C26 1.416(10) . ?
C26 N3 1.372(10) . ?
C27 H27 0.9500 . ?
C27 N3 1.371(9) . ?
C27 N4 1.336(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.548(11) . ?
C28 N3 1.457(9) . ?
C29 O2A 1.249(9) . ?
C29 O6 1.256(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 N10 1.484(7) . ?
C31 C32 1.361(9) . ?
C31 C36 1.426(9) . ?
C31 N10 1.402(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.374(10) . ?
C33 H33 0.9500 . ?
C33 C34 1.393(12) . ?
C34 H34 0.9500 . ?
C34 C35 1.374(11) . ?
C35 H35 0.9500 . ?
C35 C36 1.377(10) . ?
C36 N9 1.358(9) . ?
C37 H37 0.9500 . ?
C37 N9 1.353(9) . ?
C37 N10 1.347(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.461(12) . ?
C38 N9 1.474(8) . ?
C39 O16 1.260(12) . ?
C39 O17 1.240(10) . ?
C40 C41 1.505(9) . ?
C40 Ca0A 2.925(6) . ?
C40 O1 1.253(8) . ?
C40 O3 1.273(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 N5 1.471(8) . ?
C42 C43 1.368(9) . ?
C42 C47 1.422(9) . ?
C42 N5 1.398(9) . ?
C43 H43 0.9500 . ?
C43 C44 1.398(11) . ?
C44 H44 0.9500 . ?
C44 C45 1.394(11) . ?
C45 H45 0.9500 . ?
C45 C46 1.375(9) . ?
C46 H46 0.9500 . ?
C46 C47 1.370(10) . ?
C47 N6 1.405(8) . ?
C48 H48 0.9500 . ?
C48 N5 1.313(8) . ?
C48 N6 1.318(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.507(8) . ?
C49 N6 1.490(7) . ?
C50 C51 1.396(9) . ?
C50 C55 1.418(8) . ?
C51 C52 1.391(8) . ?
C51 C57 1.503(8) . ?
C52 C53 1.401(8) . ?
C52 C69 1.520(8) . ?
C53 C54 1.414(9) . ?
C53 C58 1.519(8) . ?
C54 C55 1.390(8) . ?
C54 C59 1.509(8) . ?
C55 C56 1.504(9) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 N8 1.484(7) . ?
C60 C61 1.368(8) . ?
C60 C65 1.405(8) . ?
C60 N8 1.406(7) . ?
C61 H61 0.9500 . ?
C61 C62 1.389(9) . ?
C62 H62 0.9500 . ?
C62 C63 1.409(9) . ?
C63 H63 0.9500 . ?
C63 C64 1.372(9) . ?
C64 H64 0.9500 . ?
C64 C65 1.378(9) . ?
C65 N7 1.398(7) . ?
C66 H66 0.9500 . ?
C66 N7 1.309(8) . ?
C66 N8 1.342(7) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.477(9) . ?
C67 N7 1.470(7) . ?
C68 O5 1.277(7) . ?
C68 O14 1.247(9) . ?
C68 Ca1B 2.833(8) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 N12 1.466(8) . ?
C70 C71 1.332(10) . ?
C70 C75 1.411(10) . ?
C70 N12 1.433(8) . ?
C71 H71 0.9500 . ?
C71 C72 1.394(13) . ?
C72 H72 0.9500 . ?
C72 C73 1.405(14) . ?
C73 H73 0.9500 . ?
C73 C74 1.402(13) . ?
C74 H74 0.9500 . ?
C74 C75 1.385(11) . ?
C75 N11 1.393(9) . ?
C76 H76 0.9500 . ?
C76 N11 1.345(9) . ?
C76 N12 1.346(8) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C77 C78 1.553(12) . ?
C77 N11 1.449(9) . ?
C78 O18 1.229(9) . ?
C78 O19 1.195(10) . ?
Ca0A Ca2 4.0098(18) . ?
Ca0A O2 2.304(4) . ?
Ca0A O1 2.705(5) . ?
Ca0A O3 2.461(5) . ?
Ca0A O5 2.351(5) . ?
Ca0A O2A 2.311(5) . ?
Ca0A O7 2.435(5) . ?
Ca0A O8 2.370(5) . ?
Ca2 O2 2.546(5) . ?
Ca2 O1 2.369(5) . ?
Ca2 O4 2.536(5) . ?
Ca2 O9 2.425(6) . ?
Ca2 O10 2.479(6) . ?
Ca2 O11 2.378(6) . ?
Ca2 O12 2.451(5) . ?
Ca2 O13 2.472(6) . ?
O5 Ca1B 2.674(6) . ?
O7 H7A 0.9034 . ?
O7 H7B 0.9036 . ?
O8 H8A 0.9559 . ?
O8 H8B 0.9550 . ?
O9 H9A 1.0509 . ?
O9 H9B 1.0480 . ?
O10 H10C 0.9996 . ?
O10 H10D 0.9946 . ?
O11 H11A 1.0337 . ?
O11 H11B 1.0345 . ?
O12 H12A 1.0057 . ?
O12 H12B 1.0064 . ?
O13 H13A 0.9787 . ?
O13 H13B 0.9752 . ?
O14 Ca1B 2.355(6) . ?
O28 H28C 0.9558 . ?
O28 H28D 0.9559 . ?
O28 Ca1B 2.446(12) . ?
O1A H1AA 1.1636 . ?
O1A H1AB 1.1806 . ?
O1A Ca1B 2.363(10) . ?

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
C2 C1 Ca2 170.7(5) . . ?
O2 C1 C2 115.1(6) . . ?
O2 C1 Ca2 62.7(3) . . ?
O4 C1 C2 120.7(5) . . ?
O4 C1 Ca2 62.2(3) . . ?
O4 C1 O2 124.3(6) . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N1 C2 C1 111.5(5) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C4 C3 C8 122.0(6) . . ?
C4 C3 N1 130.8(6) . . ?
C8 C3 N1 106.8(5) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 C3 117.4(6) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.4(6) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.3 . . ?
C7 C6 C5 121.4(6) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 H7 121.7 . . ?
C6 C7 C8 116.7(6) . . ?
C8 C7 H7 121.7 . . ?
C3 C8 C7 121.8(6) . . ?
N2 C8 C3 106.5(5) . . ?
N2 C8 C7 131.7(6) . . ?
N1 C9 H9 124.8 . . ?
N1 C9 N2 110.3(5) . . ?
N2 C9 H9 124.8 . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
N2 C10 H10A 109.0 . . ?
N2 C10 H10B 109.0 . . ?
N2 C10 C11 112.7(5) . . ?
C12 C11 C10 120.7(6) . . ?
C12 C11 C16 120.5(6) . . ?
C16 C11 C10 118.7(6) . . ?
C11 C12 C13 119.9(6) . . ?
C11 C12 C17 119.6(5) . . ?
C13 C12 C17 120.5(5) . . ?
C12 C13 C14 120.2(5) . . ?
C12 C13 C30 119.3(5) . . ?
C14 C13 C30 120.5(5) . . ?
C13 C14 C19 119.1(5) . . ?
C15 C14 C13 120.1(6) . . ?
C15 C14 C19 120.8(6) . . ?
C14 C15 C16 120.6(5) . . ?
C14 C15 C20 120.9(6) . . ?
C16 C15 C20 118.5(6) . . ?
C11 C16 C18 122.0(6) . . ?
C15 C16 C11 118.4(5) . . ?
C15 C16 C18 119.6(6) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.1 . . ?
C15 C20 H20B 109.1 . . ?
H20A C20 H20B 107.9 . . ?
N4 C20 C15 112.4(5) . . ?
N4 C20 H20A 109.1 . . ?
N4 C20 H20B 109.1 . . ?
C22 C21 C26 121.9(6) . . ?
C22 C21 N4 131.9(6) . . ?
N4 C21 C26 106.1(6) . . ?
C21 C22 H22 121.2 . . ?
C23 C22 C21 117.5(7) . . ?
C23 C22 H22 121.2 . . ?
C22 C23 H23 119.1 . . ?
C22 C23 C24 121.7(8) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.9(8) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 121.9 . . ?
C24 C25 C26 116.1(7) . . ?
C26 C25 H25 121.9 . . ?
C21 C26 C25 121.6(7) . . ?
N3 C26 C21 106.7(6) . . ?
N3 C26 C25 131.6(7) . . ?
N3 C27 H27 125.7 . . ?
N4 C27 H27 125.7 . . ?
N4 C27 N3 108.6(7) . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
N3 C28 H28A 108.2 . . ?
N3 C28 H28B 108.2 . . ?
N3 C28 C29 116.2(7) . . ?
O2A C29 C28 112.6(7) . . ?
O2A C29 O6 130.4(7) . . ?
O6 C29 C28 117.0(7) . . ?
C13 C30 H30A 109.0 . . ?
C13 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
N10 C30 C13 112.9(4) . . ?
N10 C30 H30A 109.0 . . ?
N10 C30 H30B 109.0 . . ?
C32 C31 C36 122.2(6) . . ?
C32 C31 N10 132.4(6) . . ?
N10 C31 C36 105.4(5) . . ?
C31 C32 H32 121.0 . . ?
C31 C32 C33 118.0(7) . . ?
C33 C32 H32 121.0 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.1(7) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 118.6 . . ?
C35 C34 C33 122.8(7) . . ?
C35 C34 H34 118.6 . . ?
C34 C35 H35 121.2 . . ?
C34 C35 C36 117.5(7) . . ?
C36 C35 H35 121.2 . . ?
C35 C36 C31 119.3(6) . . ?
N9 C36 C31 106.9(6) . . ?
N9 C36 C35 133.7(7) . . ?
N9 C37 H37 125.7 . . ?
N10 C37 H37 125.7 . . ?
N10 C37 N9 108.6(6) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.8 . . ?
C39 C38 H38B 108.8 . . ?
C39 C38 N9 113.8(6) . . ?
N9 C38 H38A 108.8 . . ?
N9 C38 H38B 108.8 . . ?
O16 C39 C38 118.1(7) . . ?
O17 C39 C38 118.3(8) . . ?
O17 C39 O16 123.0(9) . . ?
C41 C40 Ca0A 170.1(5) . . ?
O1 C40 C41 116.5(6) . . ?
O1 C40 Ca0A 67.5(3) . . ?
O1 C40 O3 123.6(6) . . ?
O3 C40 C41 119.8(6) . . ?
O3 C40 Ca0A 56.4(3) . . ?
C40 C41 H41A 108.7 . . ?
C40 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
N5 C41 C40 114.3(5) . . ?
N5 C41 H41A 108.7 . . ?
N5 C41 H41B 108.7 . . ?
C43 C42 C47 121.3(7) . . ?
C43 C42 N5 132.8(6) . . ?
N5 C42 C47 105.8(5) . . ?
C42 C43 H43 121.9 . . ?
C42 C43 C44 116.3(7) . . ?
C44 C43 H43 121.9 . . ?
C43 C44 H44 119.0 . . ?
C45 C44 C43 121.9(6) . . ?
C45 C44 H44 119.0 . . ?
C44 C45 H45 119.2 . . ?
C46 C45 C44 121.5(7) . . ?
C46 C45 H45 119.2 . . ?
C45 C46 H46 121.4 . . ?
C47 C46 C45 117.1(7) . . ?
C47 C46 H46 121.4 . . ?
C46 C47 C42 121.7(6) . . ?
C46 C47 N6 132.9(6) . . ?
N6 C47 C42 105.4(6) . . ?
N5 C48 H48 124.2 . . ?
N5 C48 N6 111.5(6) . . ?
N6 C48 H48 124.2 . . ?
H49A C49 H49B 108.3 . . ?
C50 C49 H49A 109.8 . . ?
C50 C49 H49B 109.8 . . ?
N6 C49 H49A 109.8 . . ?
N6 C49 H49B 109.8 . . ?
N6 C49 C50 109.3(5) . . ?
C51 C50 C49 120.6(5) . . ?
C51 C50 C55 120.8(5) . . ?
C55 C50 C49 118.6(5) . . ?
C50 C51 C57 120.0(5) . . ?
C52 C51 C50 118.7(5) . . ?
C52 C51 C57 121.3(5) . . ?
C51 C52 C53 121.9(5) . . ?
C51 C52 C69 119.4(5) . . ?
C53 C52 C69 118.6(5) . . ?
C52 C53 C54 118.3(5) . . ?
C52 C53 C58 121.3(6) . . ?
C54 C53 C58 120.4(5) . . ?
C53 C54 C59 118.3(5) . . ?
C55 C54 C53 120.7(5) . . ?
C55 C54 C59 121.0(5) . . ?
C50 C55 C56 119.1(5) . . ?
C54 C55 C50 119.2(5) . . ?
C54 C55 C56 121.7(5) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C53 C58 H58A 109.5 . . ?
C53 C58 H58B 109.5 . . ?
C53 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C54 C59 H59A 108.8 . . ?
C54 C59 H59B 108.8 . . ?
H59A C59 H59B 107.7 . . ?
N8 C59 C54 113.7(5) . . ?
N8 C59 H59A 108.8 . . ?
N8 C59 H59B 108.8 . . ?
C61 C60 C65 122.7(5) . . ?
C61 C60 N8 131.4(5) . . ?
C65 C60 N8 106.0(5) . . ?
C60 C61 H61 122.0 . . ?
C60 C61 C62 116.0(6) . . ?
C62 C61 H61 122.0 . . ?
C61 C62 H62 119.3 . . ?
C61 C62 C63 121.4(6) . . ?
C63 C62 H62 119.3 . . ?
C62 C63 H63 119.1 . . ?
C64 C63 C62 121.9(6) . . ?
C64 C63 H63 119.1 . . ?
C63 C64 H64 121.6 . . ?
C63 C64 C65 116.8(6) . . ?
C65 C64 H64 121.6 . . ?
C64 C65 C60 121.2(5) . . ?
C64 C65 N7 133.0(5) . . ?
N7 C65 C60 105.8(5) . . ?
N7 C66 H66 125.0 . . ?
N7 C66 N8 110.1(5) . . ?
N8 C66 H66 125.0 . . ?
H67A C67 H67B 107.8 . . ?
C68 C67 H67A 109.0 . . ?
C68 C67 H67B 109.0 . . ?
N7 C67 H67A 109.0 . . ?
N7 C67 H67B 109.0 . . ?
N7 C67 C68 112.7(5) . . ?
C67 C68 Ca1B 165.1(5) . . ?
O5 C68 C67 117.3(6) . . ?
O5 C68 Ca1B 69.7(4) . . ?
O14 C68 C67 119.4(6) . . ?
O14 C68 O5 123.2(7) . . ?
O14 C68 Ca1B 55.2(4) . . ?
C52 C69 H69A 109.2 . . ?
C52 C69 H69B 109.2 . . ?
H69A C69 H69B 107.9 . . ?
N12 C69 C52 112.1(5) . . ?
N12 C69 H69A 109.2 . . ?
N12 C69 H69B 109.2 . . ?
C71 C70 C75 123.7(7) . . ?
C71 C70 N12 131.3(7) . . ?
C75 C70 N12 105.0(6) . . ?
C70 C71 H71 121.7 . . ?
C70 C71 C72 116.6(9) . . ?
C72 C71 H71 121.7 . . ?
C71 C72 H72 119.6 . . ?
C71 C72 C73 120.7(8) . . ?
C73 C72 H72 119.6 . . ?
C72 C73 H73 118.7 . . ?
C74 C73 C72 122.7(8) . . ?
C74 C73 H73 118.7 . . ?
C73 C74 H74 122.7 . . ?
C75 C74 C73 114.7(8) . . ?
C75 C74 H74 122.7 . . ?
C74 C75 C70 121.6(7) . . ?
C74 C75 N11 130.7(8) . . ?
N11 C75 C70 107.8(6) . . ?
N11 C76 H76 124.9 . . ?
N11 C76 N12 110.1(6) . . ?
N12 C76 H76 124.9 . . ?
H77A C77 H77B 108.0 . . ?
C78 C77 H77A 109.4 . . ?
C78 C77 H77B 109.4 . . ?
N11 C77 H77A 109.4 . . ?
N11 C77 H77B 109.4 . . ?
N11 C77 C78 111.2(6) . . ?
O18 C78 C77 111.0(7) . . ?
O19 C78 C77 120.0(7) . . ?
O19 C78 O18 129.1(9) . . ?
C40 Ca0A Ca2 57.56(12) . . ?
O2 Ca0A C40 84.63(16) . . ?
O2 Ca0A Ca2 36.22(12) . . ?
O2 Ca0A O1 68.21(15) . . ?
O2 Ca0A O3 103.74(16) . . ?
O2 Ca0A O5 167.19(17) . . ?
O2 Ca0A O2A 89.88(17) . . ?
O2 Ca0A O7 83.04(18) . . ?
O2 Ca0A O8 103.75(19) . . ?
O1 Ca0A C40 25.33(16) . . ?
O1 Ca0A Ca2 34.93(10) . . ?
O3 Ca0A C40 25.53(17) . . ?
O3 Ca0A Ca2 82.31(12) . . ?
O3 Ca0A O1 50.78(15) . . ?
O5 Ca0A C40 103.87(17) . . ?
O5 Ca0A Ca2 156.34(13) . . ?
O5 Ca0A O1 122.96(16) . . ?
O5 Ca0A O3 81.96(17) . . ?
O5 Ca0A O7 85.99(19) . . ?
O5 Ca0A O8 86.3(2) . . ?
O2A Ca0A C40 170.5(2) . . ?
O2A Ca0A Ca2 114.03(15) . . ?
O2A Ca0A O1 145.19(19) . . ?
O2A Ca0A O3 163.58(19) . . ?
O2A Ca0A O5 82.91(19) . . ?
O2A Ca0A O7 86.79(19) . . ?
O2A Ca0A O8 85.51(19) . . ?
O7 Ca0A C40 100.24(18) . . ?
O7 Ca0A Ca2 110.35(13) . . ?
O7 Ca0A O1 115.41(17) . . ?
O7 Ca0A O3 85.84(17) . . ?
O8 Ca0A C40 88.22(19) . . ?
O8 Ca0A Ca2 79.10(13) . . ?
O8 Ca0A O1 74.61(17) . . ?
O8 Ca0A O3 99.80(19) . . ?
O8 Ca0A O7 169.71(16) . . ?
C1 Ca2 Ca0A 57.82(13) . . ?
O2 Ca2 C1 26.26(16) . . ?
O2 Ca2 Ca0A 32.33(9) . . ?
O1 Ca2 C1 96.39(18) . . ?
O1 Ca2 Ca0A 40.83(12) . . ?
O1 Ca2 O2 70.16(16) . . ?
O1 Ca2 O4 121.51(17) . . ?
O1 Ca2 O9 85.1(2) . . ?
O1 Ca2 O10 89.03(19) . . ?
O1 Ca2 O11 163.5(2) . . ?
O1 Ca2 O12 78.38(19) . . ?
O1 Ca2 O13 87.6(2) . . ?
O4 Ca2 C1 25.26(17) . . ?
O4 Ca2 Ca0A 81.87(11) . . ?
O4 Ca2 O2 51.37(14) . . ?
O9 Ca2 C1 72.68(19) . . ?
O9 Ca2 Ca0A 86.50(15) . . ?
O9 Ca2 O2 72.63(17) . . ?
O9 Ca2 O4 79.6(2) . . ?
O9 Ca2 O10 145.2(2) . . ?
O9 Ca2 O12 141.7(2) . . ?
O9 Ca2 O13 69.4(2) . . ?
O10 Ca2 C1 73.9(2) . . ?
O10 Ca2 Ca0A 67.38(15) . . ?
O10 Ca2 O2 73.07(19) . . ?
O10 Ca2 O4 74.3(2) . . ?
O11 Ca2 C1 99.6(2) . . ?
O11 Ca2 Ca0A 151.6(2) . . ?
O11 Ca2 O2 125.6(2) . . ?
O11 Ca2 O4 74.3(2) . . ?
O11 Ca2 O9 103.7(3) . . ?
O11 Ca2 O10 91.2(3) . . ?
O11 Ca2 O12 86.2(2) . . ?
O11 Ca2 O13 82.7(3) . . ?
O12 Ca2 C1 142.98(19) . . ?
O12 Ca2 Ca0A 102.16(14) . . ?
O12 Ca2 O2 130.77(17) . . ?
O12 Ca2 O4 138.2(2) . . ?
O12 Ca2 O10 69.4(2) . . ?
O12 Ca2 O13 75.52(19) . . ?
O13 Ca2 C1 141.3(2) . . ?
O13 Ca2 Ca0A 125.57(18) . . ?
O13 Ca2 O2 137.2(2) . . ?
O13 Ca2 O4 135.4(2) . . ?
O13 Ca2 O10 144.7(2) . . ?
C3 N1 C2 126.1(5) . . ?
C9 N1 C2 126.3(5) . . ?
C9 N1 C3 107.6(5) . . ?
C8 N2 C10 124.9(5) . . ?
C9 N2 C8 108.7(5) . . ?
C9 N2 C10 126.3(5) . . ?
C26 N3 C28 126.3(6) . . ?
C27 N3 C26 109.4(6) . . ?
C27 N3 C28 124.0(7) . . ?
C21 N4 C20 125.6(5) . . ?
C27 N4 C20 125.2(6) . . ?
C27 N4 C21 109.1(5) . . ?
C42 N5 C41 123.7(5) . . ?
C48 N5 C41 127.5(6) . . ?
C48 N5 C42 108.7(5) . . ?
C47 N6 C49 123.7(5) . . ?
C48 N6 C47 108.5(5) . . ?
C48 N6 C49 127.4(5) . . ?
C65 N7 C67 124.8(5) . . ?
C66 N7 C65 109.9(5) . . ?
C66 N7 C67 125.2(5) . . ?
C60 N8 C59 124.3(5) . . ?
C66 N8 C59 127.4(5) . . ?
C66 N8 C60 108.3(5) . . ?
C36 N9 C38 128.1(6) . . ?
C37 N9 C36 110.1(6) . . ?
C37 N9 C38 121.1(6) . . ?
C31 N10 C30 125.4(5) . . ?
C37 N10 C30 125.4(5) . . ?
C37 N10 C31 109.0(5) . . ?
C75 N11 C77 128.0(6) . . ?
C76 N11 C75 108.7(6) . . ?
C76 N11 C77 123.0(6) . . ?
C70 N12 C69 126.0(5) . . ?
C76 N12 C69 125.4(5) . . ?
C76 N12 C70 108.5(5) . . ?
C1 O2 Ca0A 151.5(4) . . ?
C1 O2 Ca2 91.1(4) . . ?
Ca0A O2 Ca2 111.45(18) . . ?
C40 O1 Ca0A 87.2(4) . . ?
C40 O1 Ca2 145.1(5) . . ?
Ca2 O1 Ca0A 104.24(17) . . ?
C40 O3 Ca0A 98.0(4) . . ?
C1 O4 Ca2 92.6(4) . . ?
C68 O5 Ca0A 140.2(5) . . ?
C68 O5 Ca1B 83.7(4) . . ?
Ca0A O5 Ca1B 135.5(2) . . ?
C29 O2A Ca0A 129.1(5) . . ?
Ca0A O7 H7A 125.5 . . ?
Ca0A O7 H7B 125.3 . . ?
H7A O7 H7B 109.2 . . ?
Ca0A O8 H8A 126.1 . . ?
Ca0A O8 H8B 125.5 . . ?
H8A O8 H8B 108.3 . . ?
Ca2 O9 H9A 126.7 . . ?
Ca2 O9 H9B 126.2 . . ?
H9A O9 H9B 107.2 . . ?
Ca2 O10 H10C 114.7 . . ?
Ca2 O10 H10D 114.5 . . ?
H10C O10 H10D 103.5 . . ?
Ca2 O11 H11A 126.2 . . ?
Ca2 O11 H11B 126.8 . . ?
H11A O11 H11B 106.9 . . ?
Ca2 O12 H12A 125.7 . . ?
Ca2 O12 H12B 126.3 . . ?
H12A O12 H12B 108.0 . . ?
Ca2 O13 H13A 114.1 . . ?
Ca2 O13 H13B 114.2 . . ?
H13A O13 H13B 104.4 . . ?
C68 O14 Ca1B 99.1(4) . . ?
H28C O28 H28D 108.6 . . ?
Ca1B O28 H28C 125.6 . . ?
Ca1B O28 H28D 125.8 . . ?
H1AA O1A H1AB 95.9 . . ?
Ca1B O1A H1AA 120.0 . . ?
Ca1B O1A H1AB 121.8 . . ?
O5 Ca1B C68 26.60(16) . . ?
O14 Ca1B C68 25.76(18) . . ?
O14 Ca1B O5 51.93(16) . . ?
O14 Ca1B O28 83.2(4) . . ?
O14 Ca1B O1A 130.5(3) . . ?
O28 Ca1B C68 78.1(4) . . ?
O28 Ca1B O5 69.0(3) . . ?
O1A Ca1B C68 104.8(3) . . ?
O1A Ca1B O5 79.4(3) . . ?
O1A Ca1B O28 87.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 N1 C3 68.8(8) . . . . ?
C1 C2 N1 C9 -107.2(7) . . . . ?
C2 C1 O2 Ca0A -47.0(12) . . . . ?
C2 C1 O2 Ca2 169.9(5) . . . . ?
C2 C1 O4 Ca2 -169.8(5) . . . . ?
C3 C4 C5 C6 1.1(11) . . . . ?
C3 C8 N2 C9 0.8(7) . . . . ?
C3 C8 N2 C10 177.8(6) . . . . ?
C4 C3 C8 C7 -6.4(10) . . . . ?
C4 C3 C8 N2 174.7(6) . . . . ?
C4 C3 N1 C2 8.2(11) . . . . ?
C4 C3 N1 C9 -175.2(7) . . . . ?
C4 C5 C6 C7 -1.8(12) . . . . ?
C5 C6 C7 C8 -1.5(11) . . . . ?
C6 C7 C8 C3 5.5(10) . . . . ?
C6 C7 C8 N2 -175.9(7) . . . . ?
C7 C8 N2 C9 -178.0(7) . . . . ?
C7 C8 N2 C10 -1.0(11) . . . . ?
C8 C3 C4 C5 2.8(10) . . . . ?
C8 C3 N1 C2 -178.4(6) . . . . ?
C8 C3 N1 C9 -1.8(7) . . . . ?
C10 C11 C12 C13 -174.2(5) . . . . ?
C10 C11 C12 C17 7.3(8) . . . . ?
C10 C11 C16 C15 179.1(5) . . . . ?
C10 C11 C16 C18 -4.0(8) . . . . ?
C11 C10 N2 C8 160.2(6) . . . . ?
C11 C10 N2 C9 -23.3(9) . . . . ?
C11 C12 C13 C14 -5.4(8) . . . . ?
C11 C12 C13 C30 174.9(5) . . . . ?
C12 C11 C16 C15 2.6(8) . . . . ?
C12 C11 C16 C18 179.5(5) . . . . ?
C12 C13 C14 C15 3.8(8) . . . . ?
C12 C13 C14 C19 -174.1(5) . . . . ?
C12 C13 C30 N10 98.2(6) . . . . ?
C13 C14 C15 C16 1.1(8) . . . . ?
C13 C14 C15 C20 179.5(5) . . . . ?
C13 C30 N10 C31 178.0(5) . . . . ?
C13 C30 N10 C37 3.1(9) . . . . ?
C14 C13 C30 N10 -81.6(7) . . . . ?
C14 C15 C16 C11 -4.2(8) . . . . ?
C14 C15 C16 C18 178.8(5) . . . . ?
C14 C15 C20 N4 109.9(6) . . . . ?
C15 C20 N4 C21 152.2(6) . . . . ?
C15 C20 N4 C27 -31.5(10) . . . . ?
C16 C11 C12 C13 2.1(8) . . . . ?
C16 C11 C12 C17 -176.3(5) . . . . ?
C16 C15 C20 N4 -71.6(7) . . . . ?
C17 C12 C13 C14 173.1(5) . . . . ?
C17 C12 C13 C30 -6.7(8) . . . . ?
C19 C14 C15 C16 178.9(5) . . . . ?
C19 C14 C15 C20 -2.6(8) . . . . ?
C20 C15 C16 C11 177.3(5) . . . . ?
C20 C15 C16 C18 0.3(8) . . . . ?
C21 C22 C23 C24 2.8(12) . . . . ?
C21 C26 N3 C27 -1.0(8) . . . . ?
C21 C26 N3 C28 173.2(7) . . . . ?
C22 C21 C26 C25 -4.9(11) . . . . ?
C22 C21 C26 N3 178.9(7) . . . . ?
C22 C21 N4 C20 -0.8(12) . . . . ?
C22 C21 N4 C27 -177.6(8) . . . . ?
C22 C23 C24 C25 -5.1(14) . . . . ?
C23 C24 C25 C26 2.3(13) . . . . ?
C24 C25 C26 C21 2.5(11) . . . . ?
C24 C25 C26 N3 177.7(8) . . . . ?
C25 C26 N3 C27 -176.7(8) . . . . ?
C25 C26 N3 C28 -2.6(13) . . . . ?
C26 C21 C22 C23 2.1(11) . . . . ?
C26 C21 N4 C20 178.1(6) . . . . ?
C26 C21 N4 C27 1.3(8) . . . . ?
C28 C29 O2A Ca0A -161.3(5) . . . . ?
C29 C28 N3 C26 -79.9(9) . . . . ?
C29 C28 N3 C27 93.4(10) . . . . ?
C30 C13 C14 C15 -176.5(5) . . . . ?
C30 C13 C14 C19 5.6(8) . . . . ?
C31 C32 C33 C34 0.9(11) . . . . ?
C31 C36 N9 C37 2.7(8) . . . . ?
C31 C36 N9 C38 172.5(7) . . . . ?
C32 C31 C36 C35 2.2(11) . . . . ?
C32 C31 C36 N9 179.2(6) . . . . ?
C32 C31 N10 C30 3.5(11) . . . . ?
C32 C31 N10 C37 179.1(7) . . . . ?
C32 C33 C34 C35 1.5(13) . . . . ?
C33 C34 C35 C36 -1.9(13) . . . . ?
C34 C35 C36 C31 0.1(11) . . . . ?
C34 C35 C36 N9 -175.9(8) . . . . ?
C35 C36 N9 C37 179.1(8) . . . . ?
C35 C36 N9 C38 -11.1(14) . . . . ?
C36 C31 C32 C33 -2.7(10) . . . . ?
C36 C31 N10 C30 -175.3(6) . . . . ?
C36 C31 N10 C37 0.3(7) . . . . ?
C39 C38 N9 C36 -88.6(10) . . . . ?
C39 C38 N9 C37 80.2(9) . . . . ?
C40 C41 N5 C42 66.8(8) . . . . ?
C40 C41 N5 C48 -112.2(7) . . . . ?
C41 C40 O1 Ca0A 170.1(5) . . . . ?
C41 C40 O1 Ca2 58.9(10) . . . . ?
C41 C40 O3 Ca0A -169.3(5) . . . . ?
C42 C43 C44 C45 -2.5(12) . . . . ?
C42 C47 N6 C48 -3.3(6) . . . . ?
C42 C47 N6 C49 -177.0(5) . . . . ?
C43 C42 C47 C46 -2.5(10) . . . . ?
C43 C42 C47 N6 -179.6(6) . . . . ?
C43 C42 N5 C41 2.4(11) . . . . ?
C43 C42 N5 C48 -178.5(7) . . . . ?
C43 C44 C45 C46 0.8(13) . . . . ?
C44 C45 C46 C47 0.1(12) . . . . ?
C45 C46 C47 C42 0.7(10) . . . . ?
C45 C46 C47 N6 176.9(7) . . . . ?
C46 C47 N6 C48 -180.0(7) . . . . ?
C46 C47 N6 C49 6.4(11) . . . . ?
C47 C42 C43 C44 3.3(10) . . . . ?
C47 C42 N5 C41 179.6(5) . . . . ?
C47 C42 N5 C48 -1.2(7) . . . . ?
C49 C50 C51 C52 176.6(5) . . . . ?
C49 C50 C51 C57 -2.6(8) . . . . ?
C49 C50 C55 C54 -175.2(5) . . . . ?
C49 C50 C55 C56 3.2(8) . . . . ?
C50 C49 N6 C47 -145.6(5) . . . . ?
C50 C49 N6 C48 42.0(8) . . . . ?
C50 C51 C52 C53 -3.0(8) . . . . ?
C50 C51 C52 C69 179.2(5) . . . . ?
C51 C50 C55 C54 4.5(8) . . . . ?
C51 C50 C55 C56 -177.1(5) . . . . ?
C51 C52 C53 C54 7.4(8) . . . . ?
C51 C52 C53 C58 -170.6(5) . . . . ?
C51 C52 C69 N12 76.5(7) . . . . ?
C52 C53 C54 C55 -5.9(8) . . . . ?
C52 C53 C54 C59 174.2(5) . . . . ?
C52 C69 N12 C70 -174.9(6) . . . . ?
C52 C69 N12 C76 0.8(9) . . . . ?
C53 C52 C69 N12 -101.4(6) . . . . ?
C53 C54 C55 C50 0.1(8) . . . . ?
C53 C54 C55 C56 -178.3(5) . . . . ?
C53 C54 C59 N8 100.4(6) . . . . ?
C54 C59 N8 C60 -165.5(5) . . . . ?
C54 C59 N8 C66 16.5(9) . . . . ?
C55 C50 C51 C52 -3.1(8) . . . . ?
C55 C50 C51 C57 177.8(5) . . . . ?
C55 C54 C59 N8 -79.5(7) . . . . ?
C57 C51 C52 C53 176.1(5) . . . . ?
C57 C51 C52 C69 -1.7(8) . . . . ?
C58 C53 C54 C55 172.2(5) . . . . ?
C58 C53 C54 C59 -7.8(8) . . . . ?
C59 C54 C55 C50 -180.0(5) . . . . ?
C59 C54 C55 C56 1.7(8) . . . . ?
C60 C61 C62 C63 3.2(10) . . . . ?
C60 C65 N7 C66 0.1(7) . . . . ?
C60 C65 N7 C67 175.9(6) . . . . ?
C61 C60 C65 C64 1.6(10) . . . . ?
C61 C60 C65 N7 179.9(6) . . . . ?
C61 C60 N8 C59 1.8(10) . . . . ?
C61 C60 N8 C66 -180.0(7) . . . . ?
C61 C62 C63 C64 -2.0(12) . . . . ?
C62 C63 C64 C65 0.5(11) . . . . ?
C63 C64 C65 C60 -0.2(10) . . . . ?
C63 C64 C65 N7 -178.0(7) . . . . ?
C64 C65 N7 C66 178.1(8) . . . . ?
C64 C65 N7 C67 -6.1(12) . . . . ?
C65 C60 C61 C62 -3.0(10) . . . . ?
C65 C60 N8 C59 -178.4(6) . . . . ?
C65 C60 N8 C66 -0.2(7) . . . . ?
C67 C68 O5 Ca0A 23.4(12) . . . . ?
C67 C68 O5 Ca1B -165.7(6) . . . . ?
C67 C68 O14 Ca1B 163.6(6) . . . . ?
C68 C67 N7 C65 -71.4(8) . . . . ?
C68 C67 N7 C66 103.7(7) . . . . ?
C69 C52 C53 C54 -174.7(5) . . . . ?
C69 C52 C53 C58 7.2(8) . . . . ?
C70 C71 C72 C73 -2.4(14) . . . . ?
C70 C75 N11 C76 -0.1(9) . . . . ?
C70 C75 N11 C77 -174.2(7) . . . . ?
C71 C70 C75 C74 1.6(13) . . . . ?
C71 C70 C75 N11 -178.0(7) . . . . ?
C71 C70 N12 C69 -5.7(12) . . . . ?
C71 C70 N12 C76 178.0(8) . . . . ?
C71 C72 C73 C74 1.8(16) . . . . ?
C72 C73 C74 C75 0.6(14) . . . . ?
C73 C74 C75 C70 -2.2(13) . . . . ?
C73 C74 C75 N11 177.3(9) . . . . ?
C74 C75 N11 C76 -179.6(9) . . . . ?
C74 C75 N11 C77 6.3(14) . . . . ?
C75 C70 C71 C72 0.8(12) . . . . ?
C75 C70 N12 C69 176.6(6) . . . . ?
C75 C70 N12 C76 0.3(8) . . . . ?
C78 C77 N11 C75 109.8(9) . . . . ?
C78 C77 N11 C76 -63.6(10) . . . . ?
Ca0A C40 O1 Ca2 -111.1(7) . . . . ?
Ca2 C1 O2 Ca0A 143.1(10) . . . . ?
N1 C3 C4 C5 175.3(7) . . . . ?
N1 C3 C8 C7 179.6(6) . . . . ?
N1 C3 C8 N2 0.6(7) . . . . ?
N1 C9 N2 C8 -2.1(7) . . . . ?
N1 C9 N2 C10 -179.0(6) . . . . ?
N2 C9 N1 C2 179.0(6) . . . . ?
N2 C9 N1 C3 2.4(7) . . . . ?
N2 C10 C11 C12 -95.0(7) . . . . ?
N2 C10 C11 C16 88.6(7) . . . . ?
N3 C27 N4 C20 -178.7(6) . . . . ?
N3 C27 N4 C21 -2.0(9) . . . . ?
N3 C28 C29 O2A -174.8(7) . . . . ?
N3 C28 C29 O6 6.8(11) . . . . ?
N4 C21 C22 C23 -179.1(8) . . . . ?
N4 C21 C26 C25 176.0(7) . . . . ?
N4 C21 C26 N3 -0.2(8) . . . . ?
N4 C27 N3 C26 1.8(9) . . . . ?
N4 C27 N3 C28 -172.5(7) . . . . ?
N5 C42 C43 C44 -179.8(7) . . . . ?
N5 C42 C47 C46 179.8(6) . . . . ?
N5 C42 C47 N6 2.7(6) . . . . ?
N5 C48 N6 C47 2.7(7) . . . . ?
N5 C48 N6 C49 176.1(5) . . . . ?
N6 C48 N5 C41 178.2(6) . . . . ?
N6 C48 N5 C42 -0.9(7) . . . . ?
N6 C49 C50 C51 -103.3(6) . . . . ?
N6 C49 C50 C55 76.4(6) . . . . ?
N7 C66 N8 C59 178.4(6) . . . . ?
N7 C66 N8 C60 0.2(7) . . . . ?
N7 C67 C68 O5 -169.8(6) . . . . ?
N7 C67 C68 O14 10.5(10) . . . . ?
N7 C67 C68 Ca1B 74.9(19) . . . . ?
N8 C60 C61 C62 176.8(6) . . . . ?
N8 C60 C65 C64 -178.3(6) . . . . ?
N8 C60 C65 N7 0.0(7) . . . . ?
N8 C66 N7 C65 -0.2(8) . . . . ?
N8 C66 N7 C67 -176.0(6) . . . . ?
N9 C37 N10 C30 177.0(6) . . . . ?
N9 C37 N10 C31 1.4(8) . . . . ?
N9 C38 C39 O16 11.6(12) . . . . ?
N9 C38 C39 O17 -176.8(7) . . . . ?
N10 C31 C32 C33 178.6(7) . . . . ?
N10 C31 C36 C35 -178.8(6) . . . . ?
N10 C31 C36 N9 -1.8(7) . . . . ?
N10 C37 N9 C36 -2.6(8) . . . . ?
N10 C37 N9 C38 -173.3(6) . . . . ?
N11 C76 N12 C69 -176.7(6) . . . . ?
N11 C76 N12 C70 -0.3(8) . . . . ?
N11 C77 C78 O18 -159.2(9) . . . . ?
N11 C77 C78 O19 21.2(12) . . . . ?
N12 C70 C71 C72 -176.5(8) . . . . ?
N12 C70 C75 C74 179.5(7) . . . . ?
N12 C70 C75 N11 -0.1(8) . . . . ?
N12 C76 N11 C75 0.3(8) . . . . ?
N12 C76 N11 C77 174.7(6) . . . . ?
O2 C1 C2 N1 176.2(5) . . . . ?
O2 C1 O4 Ca2 9.0(7) . . . . ?
O1 C40 C41 N5 178.1(6) . . . . ?
O1 C40 O3 Ca0A 7.0(7) . . . . ?
O3 C40 C41 N5 -5.4(9) . . . . ?
O3 C40 O1 Ca0A -6.3(7) . . . . ?
O3 C40 O1 Ca2 -117.4(8) . . . . ?
O4 C1 C2 N1 -4.8(9) . . . . ?
O4 C1 O2 Ca0A 134.1(8) . . . . ?
O4 C1 O2 Ca2 -9.0(7) . . . . ?
O5 C68 O14 Ca1B -16.1(9) . . . . ?
O14 C68 O5 Ca0A -156.8(6) . . . . ?
O14 C68 O5 Ca1B 14.1(8) . . . . ?
O6 C29 O2A Ca0A 16.8(13) . . . . ?
Ca1B C68 O5 Ca0A -170.9(8) . . . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.054 0.446 1710 114 ' '
2 0.157 0.489 0.423 15 1 ' '
3 0.843 0.511 0.577 15 1 ' '
_platon_squeeze_details          
;
Approximately 30% of the unit cell volume comprises a 
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 114 electrons per unit cell.
 


TITL exp_2409  P -1         R = 0.11
CELL   14.3416   20.7798   21.1629     89.72     74.47     75.25
SPGR P-1
# Solvent Accessible Volume =    1742.4
# Electrons Found in S.A.V. =     112.9
# Note: Atoms in Void as Cxxx and Qxxx all others
Q101 1.000 0.500 0.500 !       3.79 eA-3
Q102 0.579 0.466 0.219 !       2.90 eA-3
Q103 0.764 0.590 0.727 !       2.78 eA-3
Q104 0.515 0.976 0.736 !       2.56 eA-3
Q105 0.876 0.505 0.751 !       2.36 eA-3
Q106 0.499 0.262 0.260 !       2.18 eA-3
Q107 0.113 0.422 0.199 !       2.15 eA-3
Q108 0.279 0.476 0.259 !       2.04 eA-3
Q109 0.702 0.544 0.730 !       1.91 eA-3
Q110 0.285 0.250 0.530 !       1.78 eA-3
Q111 0.160 0.340 0.261 !       1.70 eA-3
Q112 0.015 0.927 0.956 !       1.56 eA-3
Q113 0.656 0.217 0.987 !       1.39 eA-3
Q114 0.782 0.232 0.103 !       1.30 eA-3
Q115 0.202 0.886 0.770 !       1.09 eA-3
Q116 0.751 0.393 0.619 !       1.02 eA-3
Q117 0.841 0.638 0.605 !       1.01 eA-3
Q118 0.722 0.646 0.643 !       0.97 eA-3
Q119 0.173 0.380 0.282 !       0.95 eA-3
Q120 0.185 0.427 0.244 !       0.95 eA-3
Q121 0.405 0.323 0.699 !       0.95 eA-3
Q122 0.751 0.651 0.621 !       0.95 eA-3
Q123 0.122 0.333 0.667 !       0.93 eA-3
Q124 0.840 0.876 0.120 !       0.93 eA-3
Q125 0.104 0.838 0.185 !       0.93 eA-3
Q126 0.282 0.393 0.324 !       0.91 eA-3
Q127 0.596 0.745 0.298 !       0.90 eA-3
Q128 0.643 0.268 0.407 !       0.90 eA-3
Q129 0.111 0.927 0.018 !       0.90 eA-3
Q130 0.562 0.601 0.530 !       0.90 eA-3
Q131 0.388 0.045 0.110 !       0.88 eA-3
Q132 0.641 0.255 0.572 !       0.84 eA-3
Q133 0.920 0.183 0.829 !       0.84 eA-3
Q134 0.594 0.266 0.796 !       0.82 eA-3
C135 0.064 0.024 0.368 !       0.82 eA-3
Q136 0.546 0.209 0.637 !       0.81 eA-3
Q137 0.783 0.203 0.758 !       0.81 eA-3
C138 0.205 0.631 0.830 !       0.81 eA-3
Q139 0.592 0.123 0.624 !       0.79 eA-3
Q140 0.551 0.657 0.797 !       0.79 eA-3
Q141 0.247 0.300 0.233 !       0.79 eA-3
Q142 0.348 0.264 0.737 !       0.76 eA-3
Q143 0.309 0.422 0.312 !       0.76 eA-3
Q144 0.451 0.083 0.033 !       0.75 eA-3
C145 0.833 0.921 0.639 !       0.74 eA-3
Q146 0.209 0.401 0.231 !       0.74 eA-3
Q147 0.187 0.313 0.748 !       0.74 eA-3
Q148 0.841 0.708 0.232 !       0.74 eA-3
Q149 0.467 0.278 0.881 !       0.73 eA-3
Q150 0.516 0.097 0.037 !       0.73 eA-3
Q151 0.299 0.974 0.764 !       0.73 eA-3
C152 0.906 0.136 0.435 !       0.73 eA-3
C153 0.083 0.783 0.980 !       0.73 eA-3
C154 0.949 0.182 0.514 !       0.73 eA-3
Q155 0.688 0.653 0.868 !       0.72 eA-3
Q156 0.531 0.685 0.144 !       0.72 eA-3
Q157 0.076 0.301 0.665 !       0.72 eA-3
C158 0.125 0.945 0.397 !       0.72 eA-3
Q159 0.064 0.309 0.790 !       0.71 eA-3
Q160 0.469 0.702 0.163 !       0.71 eA-3
Q161 0.579 0.126 0.528 !       0.71 eA-3
Q162 0.766 0.722 0.232 !       0.70 eA-3
Q163 0.159 0.109 0.968 !       0.70 eA-3
C164 0.812 0.952 0.699 !       0.70 eA-3
Q165 0.364 0.205 0.282 !       0.70 eA-3
Q166 0.220 0.635 0.924 !       0.69 eA-3
Q167 0.362 0.203 0.308 !       0.69 eA-3
Q168 0.597 0.310 0.203 !       0.69 eA-3
Q169 0.265 0.248 0.395 !       0.69 eA-3
Q170 0.859 0.731 0.483 !       0.69 eA-3
C171 0.845 0.394 0.129 !       0.68 eA-3
Q172 0.095 0.926 0.952 !       0.68 eA-3
Q173 0.376 0.343 0.201 !       0.68 eA-3
Q174 0.432 0.563 0.607 !       0.68 eA-3
Q175 0.080 1.002 0.030 !       0.68 eA-3
C176 0.968 0.661 0.986 !       0.68 eA-3
Q177 0.530 0.685 0.339 !       0.68 eA-3
Q178 0.982 0.690 0.139 !       0.68 eA-3
Q179 0.470 0.812 0.174 !       0.68 eA-3
Q180 0.630 0.243 0.932 !       0.68 eA-3
Q181 0.575 0.598 0.957 !       0.67 eA-3
Q182 0.448 0.733 0.375 !       0.67 eA-3
Q183 0.048 0.831 0.261 !       0.67 eA-3
Q184 0.912 0.078 0.720 !       0.67 eA-3
Q185 0.482 0.815 0.338 !       0.67 eA-3
Q186 0.064 0.434 0.498 !       0.67 eA-3
Q187 0.360 0.855 0.642 !       0.67 eA-3
Q188 0.922 0.367 0.747 !       0.67 eA-3
Q189 0.234 0.750 0.644 !       0.67 eA-3
Q190 0.454 0.371 0.071 !       0.66 eA-3
Q191 0.331 0.258 0.935 !       0.66 eA-3
Q192 0.641 0.230 0.786 !       0.66 eA-3
Q193 0.485 0.202 0.655 !       0.65 eA-3
Q194 0.267 0.862 0.860 !       0.65 eA-3
Q195 0.721 0.957 0.654 !       0.65 eA-3
C196 0.952 0.999 0.675 !       0.65 eA-3
Q197 0.499 0.614 0.439 !       0.65 eA-3
Q198 0.438 0.241 0.877 !       0.65 eA-3
C199 0.120 0.079 0.367 !       0.65 eA-3
(replace by semicolon in column 1 when used as .sqf)
;
_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
