# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_mo_40626ca
_database_code_depnum_ccdc_archive 'CCDC 1505410'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C55 H88 Ca2 Cl4 N20 O21'
_chemical_formula_weight         1587.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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                   15.086(4)
_cell_length_b                   17.048(4)
_cell_length_c                   17.876(8)
_cell_angle_alpha                103.160(5)
_cell_angle_beta                 110.463(6)
_cell_angle_gamma                107.684(4)
_cell_volume                     3806(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9823
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.33

_exptl_crystal_description       polyhedral
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_F_000             1668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    0.371
_shelx_estimated_absorpt_T_min   0.808
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23780
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.311
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             14662
_reflns_number_gt                10021
_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_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.2000P)²] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14662
_refine_ls_number_parameters     919
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_gt           0.1187
_refine_ls_wR_factor_ref         0.3927
_refine_ls_wR_factor_gt          0.3621
_refine_ls_goodness_of_fit_ref   1.483
_refine_ls_restrained_S_all      1.483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.500 0.500 272.7 43.5
2 0.299 0.530 0.649 9.1 0.5
3 0.489 0.369 0.071 70.2 16.5
4 0.511 0.631 0.929 70.2 16.7
5 0.701 0.470 0.351 9.1 1.3
_platon_squeeze_details          
; 
;

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
Ca1 Ca -0.06518(8) 0.90308(7) 0.21489(8) 0.0267(3) Uani 1 1 d . . . . .
Ca2 Ca 0.20864(8) 0.74119(7) 0.25280(7) 0.0251(3) Uani 1 1 d . . . . .
Cl1 Cl 0.07026(11) 0.82024(9) 0.23451(10) 0.0357(4) Uani 1 1 d . . . . .
Cl2 Cl 0.1635(2) 0.84971(15) 0.68604(14) 0.0683(6) Uani 1 1 d . . . . .
Cl3 Cl 0.72698(19) 0.52924(13) 0.76119(15) 0.0706(7) Uani 1 1 d . . . . .
Cl4 Cl 0.6882(2) 0.96285(16) 0.01972(15) 0.0701(6) Uani 1 1 d . . . . .
O1 O 0.0384(3) 1.0011(2) 0.3697(3) 0.0269(9) Uani 1 1 d . . . . .
O2 O 0.3111(3) 0.8439(2) 0.4066(3) 0.0280(9) Uani 1 1 d . . . . .
O3 O 0.0709(3) 1.0296(2) 0.2241(3) 0.0324(10) Uani 1 1 d . . . . .
O4 O 0.3395(3) 0.8764(2) 0.2651(3) 0.0258(8) Uani 1 1 d . . . . .
O5 O -0.0830(3) 0.8851(2) 0.0664(3) 0.0315(9) Uani 1 1 d . . . . .
O6 O 0.1823(3) 0.7263(2) 0.1083(3) 0.0303(9) Uani 1 1 d . . . . .
O7 O -0.2111(3) 0.7569(2) 0.1131(3) 0.0343(10) Uani 1 1 d . . . . .
O8 O 0.0584(3) 0.5952(3) 0.1496(3) 0.0340(10) Uani 1 1 d . . . . .
O9 O -0.1298(3) 0.8273(2) 0.2986(3) 0.0307(9) Uani 1 1 d . . . . .
O10 O 0.1352(3) 0.6698(3) 0.3348(3) 0.0335(10) Uani 1 1 d . . . . .
O11 O -0.1731(4) 0.9755(3) 0.1993(3) 0.0469(12) Uani 1 1 d . . . . .
O12 O 0.3239(3) 0.6735(3) 0.2819(3) 0.0422(11) Uani 1 1 d . . . . .
N1 N 0.1141(3) 0.9541(3) 0.4749(3) 0.0238(10) Uani 1 1 d . . . . .
N2 N 0.2162(3) 1.0565(3) 0.4365(3) 0.0232(10) Uani 1 1 d . . . . .
N3 N 0.3379(3) 0.9878(3) 0.4555(3) 0.0248(10) Uani 1 1 d . . . . .
N4 N 0.2338(3) 0.8833(3) 0.4879(3) 0.0241(10) Uani 1 1 d . . . . .
N5 N 0.2432(4) 1.0864(3) 0.3154(3) 0.0288(11) Uani 1 1 d . . . . .
N6 N 0.1828(4) 1.0278(3) 0.1660(3) 0.0290(11) Uani 1 1 d . . . . .
N7 N 0.3046(4) 0.9588(3) 0.1843(3) 0.0275(10) Uani 1 1 d . . . . .
N8 N 0.3669(3) 1.0180(3) 0.3332(3) 0.0256(10) Uani 1 1 d . . . . .
N9 N 0.0506(4) 0.9014(3) 0.0306(3) 0.0280(11) Uani 1 1 d . . . . .
N10 N -0.0896(4) 0.7642(3) -0.0254(3) 0.0306(11) Uani 1 1 d . . . . .
N11 N 0.0292(4) 0.6935(3) -0.0052(3) 0.0276(11) Uani 1 1 d . . . . .
N12 N 0.1708(4) 0.8319(3) 0.0512(3) 0.0306(11) Uani 1 1 d . . . . .
N13 N -0.1919(4) 0.6574(3) 0.0178(3) 0.0324(12) Uani 1 1 d . . . . .
N14 N -0.2197(4) 0.6286(3) 0.1320(3) 0.0307(11) Uani 1 1 d . . . . .
N15 N -0.1016(4) 0.5545(3) 0.1471(3) 0.0324(12) Uani 1 1 d . . . . .
N16 N -0.0766(4) 0.5826(3) 0.0317(3) 0.0292(11) Uani 1 1 d . . . . .
N17 N -0.1569(4) 0.6855(3) 0.2903(3) 0.0328(12) Uani 1 1 d . . . . .
N18 N -0.0310(4) 0.8061(3) 0.4158(3) 0.0272(10) Uani 1 1 d . . . . .
N19 N 0.0884(4) 0.7368(3) 0.4319(3) 0.0287(11) Uani 1 1 d . . . . .
N20 N -0.0363(4) 0.6153(3) 0.3050(3) 0.0308(11) Uani 1 1 d . . . . .
C1 C 0.1178(4) 1.0023(3) 0.4229(4) 0.0270(12) Uani 1 1 d . . . . .
C2 C 0.3113(4) 1.0566(3) 0.4966(4) 0.0262(12) Uani 1 1 d . . . . .
H2 H 0.3700 1.1159 0.5171 0.031 Uiso 1 1 calc R U . . .
C3 C 0.2936(4) 0.9014(3) 0.4470(4) 0.0245(12) Uani 1 1 d . . . . .
C4 C 0.2087(4) 0.9501(3) 0.5352(4) 0.0258(12) Uani 1 1 d . . . . .
H4 H 0.1956 0.9332 0.5817 0.031 Uiso 1 1 calc R U . . .
C5 C 0.2259(4) 1.1165(4) 0.3896(4) 0.0292(13) Uani 1 1 d . . . . .
H5A H 0.1614 1.1262 0.3702 0.035 Uiso 1 1 calc R U . . .
H5B H 0.2844 1.1746 0.4301 0.035 Uiso 1 1 calc R U . . .
C6 C 0.4084(4) 1.0116(4) 0.4183(4) 0.0269(12) Uani 1 1 d . . . . .
H6A H 0.4383 0.9675 0.4141 0.032 Uiso 1 1 calc R U . . .
H6B H 0.4667 1.0697 0.4592 0.032 Uiso 1 1 calc R U . . .
C7 C 0.1608(4) 1.0463(3) 0.2346(4) 0.0283(13) Uani 1 1 d . . . . .
C8 C 0.2862(4) 1.0375(4) 0.1760(4) 0.0289(12) Uani 1 1 d . . . . .
H8 H 0.2931 1.0461 0.1245 0.035 Uiso 1 1 calc R U . . .
C9 C 0.3354(4) 0.9469(4) 0.2610(4) 0.0250(12) Uani 1 1 d . . . . .
C10 C 0.3498(4) 1.0981(4) 0.3296(4) 0.0309(13) Uani 1 1 d . . . . .
H10 H 0.4009 1.1486 0.3854 0.037 Uiso 1 1 calc R U . . .
C11 C 0.0996(4) 0.9983(4) 0.0794(4) 0.0312(13) Uani 1 1 d . . . . .
H11A H 0.1282 1.0287 0.0466 0.037 Uiso 1 1 calc R U . . .
H11B H 0.0449 1.0171 0.0837 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2801(4) 0.8887(4) 0.1056(4) 0.0288(12) Uani 1 1 d . . . . .
H12A H 0.3088 0.9168 0.0714 0.035 Uiso 1 1 calc R U . . .
H12B H 0.3164 0.8512 0.1220 0.035 Uiso 1 1 calc R U . . .
C13 C -0.0416(4) 0.8523(4) 0.0269(4) 0.0286(13) Uani 1 1 d . . . . .
C14 C -0.0369(5) 0.7220(4) -0.0646(4) 0.0324(14) Uani 1 1 d . . . . .
H14 H -0.0913 0.6684 -0.1169 0.039 Uiso 1 1 calc R U . . .
C15 C 0.1302(4) 0.7496(4) 0.0553(4) 0.0287(12) Uani 1 1 d . . . . .
C16 C 0.1074(4) 0.8625(4) -0.0092(4) 0.0310(13) Uani 1 1 d . . . . .
H16 H 0.1542 0.9088 -0.0207 0.037 Uiso 1 1 calc R U . . .
C17 C -0.1927(4) 0.7098(4) -0.0357(4) 0.0322(14) Uani 1 1 d . . . . .
H17A H -0.2260 0.7495 -0.0225 0.039 Uiso 1 1 calc R U . . .
H17B H -0.2366 0.6692 -0.0968 0.039 Uiso 1 1 calc R U . . .
C18 C -0.0127(4) 0.6011(4) -0.0119(4) 0.0311(13) Uani 1 1 d . . . . .
H18A H -0.0547 0.5622 -0.0736 0.037 Uiso 1 1 calc R U . . .
H18B H 0.0464 0.5853 0.0120 0.037 Uiso 1 1 calc R U . . .
C19 C -0.2060(4) 0.6838(3) 0.0899(4) 0.0289(13) Uani 1 1 d . . . . .
C20 C -0.2116(4) 0.5429(3) 0.1065(4) 0.0315(13) Uani 1 1 d . . . . .
H20 H -0.2535 0.5012 0.1251 0.038 Uiso 1 1 calc R U . . .
C21 C -0.0351(4) 0.5797(3) 0.1126(4) 0.0295(13) Uani 1 1 d . . . . .
C22 C -0.1864(4) 0.5717(3) -0.0113(4) 0.0316(14) Uani 1 1 d . . . . .
H22 H -0.2107 0.5508 -0.0749 0.038 Uiso 1 1 calc R U . . .
C23 C -0.2447(4) 0.6499(4) 0.2048(4) 0.0332(14) Uani 1 1 d . . . . .
H23A H -0.2752 0.6935 0.2005 0.040 Uiso 1 1 calc R U . . .
H23B H -0.2988 0.5952 0.1991 0.040 Uiso 1 1 calc R U . . .
C24 C -0.0622(5) 0.5416(4) 0.2280(4) 0.0358(14) Uani 1 1 d . . . . .
H24A H 0.0011 0.5314 0.2358 0.043 Uiso 1 1 calc R U . . .
H24B H -0.1152 0.4871 0.2237 0.043 Uiso 1 1 calc R U . . .
C25 C -0.1073(4) 0.7763(4) 0.3316(4) 0.0285(13) Uani 1 1 d . . . . .
C26 C 0.0061(4) 0.7468(4) 0.4532(4) 0.0322(13) Uani 1 1 d . . . . .
H26 H 0.0354 0.7738 0.5172 0.039 Uiso 1 1 calc R U . . .
C27 C 0.0660(5) 0.6749(4) 0.3558(4) 0.0294(12) Uani 1 1 d . . . . .
C28 C -0.1206(5) 0.6247(4) 0.3238(4) 0.0337(14) Uani 1 1 d . . . . .
H28 H -0.1805 0.5650 0.2972 0.040 Uiso 1 1 calc R U . . .
C29 C 0.0127(4) 0.9002(4) 0.4685(4) 0.0283(13) Uani 1 1 d . . . . .
H29A H 0.0211 0.9059 0.5272 0.034 Uiso 1 1 calc R U . . .
H29B H -0.0376 0.9245 0.4442 0.034 Uiso 1 1 calc R U . . .
C30 C 0.1983(4) 0.7953(4) 0.4908(4) 0.0269(12) Uani 1 1 d . . . . .
H30A H 0.2099 0.8015 0.5502 0.032 Uiso 1 1 calc R U . . .
H30B H 0.2417 0.7665 0.4771 0.032 Uiso 1 1 calc R U . . .
C31 C 0.2998(4) 1.0417(4) 0.5754(4) 0.0266(12) Uani 1 1 d . . . . .
C32 C 0.2771(5) 1.1138(4) 0.6256(4) 0.0365(15) Uani 1 1 d . . . . .
H32A H 0.2714 1.1567 0.5971 0.044 Uiso 1 1 calc R U . . .
H32B H 0.2111 1.0864 0.6287 0.044 Uiso 1 1 calc R U . . .
C33 C 0.3675(6) 1.1592(6) 0.7140(6) 0.072(3) Uani 1 1 d . . . . .
H33A H 0.3450 1.1804 0.7574 0.086 Uiso 1 1 calc R U . . .
H33B H 0.4230 1.2106 0.7164 0.086 Uiso 1 1 calc R U . . .
C34 C 0.4070(6) 1.0894(7) 0.7306(5) 0.063(3) Uani 1 1 d . . . . .
H34A H 0.3614 1.0467 0.7453 0.076 Uiso 1 1 calc R U . . .
H34B H 0.4794 1.1169 0.7771 0.076 Uiso 1 1 calc R U . . .
C35 C 0.4007(4) 1.0449(4) 0.6424(4) 0.0332(14) Uani 1 1 d . . . . .
H35A H 0.3967 0.9843 0.6343 0.040 Uiso 1 1 calc R U . . .
H35B H 0.4624 1.0801 0.6374 0.040 Uiso 1 1 calc R U . . .
C36 C 0.3703(5) 1.1201(4) 0.2575(5) 0.0367(15) Uani 1 1 d . . . . .
C37 C 0.3572(6) 1.2047(4) 0.2481(5) 0.0459(17) Uani 1 1 d . . . . .
H37A H 0.2825 1.1914 0.2169 0.055 Uiso 1 1 calc R U . . .
H37B H 0.3875 1.2520 0.3054 0.055 Uiso 1 1 calc R U . . .
C38 C 0.4135(9) 1.2327(7) 0.1989(8) 0.080(3) Uani 1 1 d . . . . .
H38A H 0.4445 1.2982 0.2176 0.096 Uiso 1 1 calc R U . . .
H38B H 0.3653 1.2067 0.1365 0.096 Uiso 1 1 calc R U . . .
C39 C 0.5015(7) 1.1977(7) 0.2182(7) 0.068(2) Uani 1 1 d . . . . .
H39A H 0.4988 1.1640 0.1638 0.081 Uiso 1 1 calc R U . . .
H39B H 0.5712 1.2480 0.2533 0.081 Uiso 1 1 calc R U . . .
C40 C 0.4808(5) 1.1377(5) 0.2672(5) 0.0463(17) Uani 1 1 d . . . . .
H40A H 0.5326 1.1673 0.3287 0.056 Uiso 1 1 calc R U . . .
H40B H 0.4847 1.0813 0.2426 0.056 Uiso 1 1 calc R U . . .
C41 C 0.0303(5) 0.7851(4) -0.0926(4) 0.0369(15) Uani 1 1 d . . . . .
C42 C -0.0361(6) 0.8142(5) -0.1587(5) 0.0449(17) Uani 1 1 d . . . . .
H42A H 0.0044 0.8758 -0.1510 0.054 Uiso 1 1 calc R U . . .
H42B H -0.0996 0.8110 -0.1522 0.054 Uiso 1 1 calc R U . . .
C43 C -0.0653(8) 0.7479(6) -0.2482(5) 0.067(2) Uani 1 1 d . . . . .
H43A H -0.1405 0.7076 -0.2777 0.080 Uiso 1 1 calc R U . . .
H43B H -0.0497 0.7802 -0.2847 0.080 Uiso 1 1 calc R U . . .
C44 C -0.0014(7) 0.6964(6) -0.2320(6) 0.062(2) Uani 1 1 d . . . . .
H44A H 0.0319 0.6940 -0.2709 0.074 Uiso 1 1 calc R U . . .
H44B H -0.0457 0.6349 -0.2422 0.074 Uiso 1 1 calc R U . . .
C45 C 0.0808(5) 0.7435(5) -0.1392(5) 0.0429(16) Uani 1 1 d . . . . .
H45A H 0.1007 0.7009 -0.1156 0.051 Uiso 1 1 calc R U . . .
H45B H 0.1438 0.7895 -0.1340 0.051 Uiso 1 1 calc R U . . .
C46 C -0.2555(4) 0.5026(4) 0.0082(4) 0.0344(14) Uani 1 1 d . . . . .
C47 C -0.3719(5) 0.4872(4) -0.0367(5) 0.0401(16) Uani 1 1 d . . . . .
H47A H -0.4033 0.4845 0.0035 0.048 Uiso 1 1 calc R U . . .
H47B H -0.3779 0.5355 -0.0571 0.048 Uiso 1 1 calc R U . . .
C48 C -0.4259(6) 0.3980(5) -0.1129(6) 0.060(2) Uani 1 1 d . . . . .
H48A H -0.5007 0.3683 -0.1282 0.072 Uiso 1 1 calc R U . . .
H48B H -0.4191 0.4061 -0.1640 0.072 Uiso 1 1 calc R U . . .
C49 C -0.3679(6) 0.3451(5) -0.0795(6) 0.057(2) Uani 1 1 d . . . . .
H49A H -0.3953 0.3180 -0.0443 0.069 Uiso 1 1 calc R U . . .
H49B H -0.3753 0.2974 -0.1279 0.069 Uiso 1 1 calc R U . . .
C50 C -0.2560(5) 0.4104(4) -0.0258(5) 0.0389(15) Uani 1 1 d . . . . .
H50A H -0.2178 0.4111 -0.0610 0.047 Uiso 1 1 calc R U . . .
H50B H -0.2220 0.3941 0.0228 0.047 Uiso 1 1 calc R U . . .
C51 C -0.0826(5) 0.6590(4) 0.4210(5) 0.0424(16) Uani 1 1 d . . . . .
C52 C -0.1671(5) 0.6640(5) 0.4470(5) 0.0464(17) Uani 1 1 d . . . . .
H52A H -0.1573 0.7265 0.4680 0.056 Uiso 1 1 calc R U . . .
H52B H -0.2364 0.6292 0.3965 0.056 Uiso 1 1 calc R U . . .
C53 C -0.1618(15) 0.6297(13) 0.5126(13) 0.145(7) Uani 1 1 d D . . . .
H53A H -0.2324 0.5869 0.4977 0.174 Uiso 1 1 calc R U . . .
H53B H -0.1371 0.6788 0.5674 0.174 Uiso 1 1 calc R U . . .
C54 C -0.0916(11) 0.5856(11) 0.5239(10) 0.102(4) Uani 1 1 d D . . . .
H54A H -0.1300 0.5224 0.5130 0.123 Uiso 1 1 calc R U . . .
H54B H -0.0343 0.6145 0.5834 0.123 Uiso 1 1 calc R U . . .
C55 C -0.0483(6) 0.5934(5) 0.4595(5) 0.0493(18) Uani 1 1 d D . . . .
H55A H -0.0768 0.5347 0.4134 0.059 Uiso 1 1 calc R U . . .
H55B H 0.0287 0.6167 0.4885 0.059 Uiso 1 1 calc R U . . .
O13 O 0.6454(7) 0.0920(6) 0.1378(7) 0.121(3) Uani 1 1 d . . . . .
O14 O 0.5117(10) 0.5124(9) 0.2895(9) 0.162(5) Uani 1 1 d . . . . .
O15 O 0.5530(11) 0.4431(10) 0.4126(9) 0.162(5) Uani 1 1 d . . . . .
O16 O 0.4826(8) 0.1692(7) 0.9614(8) 0.134(4) Uani 1 1 d . . . . .
O17 O 0.6848(9) 0.3626(7) 0.4548(8) 0.167(6) Uani 1 1 d . . . . .
O18 O 0.7909(9) 0.3270(7) 0.3539(9) 0.162(6) Uani 1 1 d . . . . .
O19 O 0.8099(7) 0.4629(6) 0.6249(6) 0.103(3) Uani 1 1 d . . . . .
O20 O 0.2734(4) 0.6220(4) 0.7866(5) 0.089(3) Uani 1 1 d . . . . .
O21 O 0.3413(6) 0.7860(7) 0.9205(7) 0.114(3) 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 O11 2.306(4) . ?
Ca1 O3 2.409(4) . ?
Ca1 O9 2.448(5) . ?
Ca1 O7 2.484(4) . ?
Ca1 O1 2.485(4) . ?
Ca1 O5 2.509(5) . ?
Ca1 Cl1 2.7874(17) . ?
Ca2 O12 2.341(4) . ?
Ca2 O6 2.411(5) . ?
Ca2 O4 2.441(4) . ?
Ca2 O10 2.446(5) . ?
Ca2 O2 2.491(4) . ?
Ca2 O8 2.509(4) . ?
Ca2 Cl1 2.7774(17) . ?
O1 C1 1.233(7) . ?
O2 C3 1.235(6) . ?
O3 C7 1.233(7) . ?
O4 C9 1.240(7) . ?
O5 C13 1.241(7) . ?
O6 C15 1.229(7) . ?
O7 C19 1.255(7) . ?
O8 C21 1.241(7) . ?
O9 C25 1.223(7) . ?
O10 C27 1.246(7) . ?
N1 C1 1.378(8) . ?
N1 C29 1.473(7) . ?
N1 C4 1.491(7) . ?
N2 C1 1.389(7) . ?
N2 C2 1.460(7) . ?
N2 C5 1.469(8) . ?
N3 C3 1.367(7) . ?
N3 C6 1.448(8) . ?
N3 C2 1.474(6) . ?
N4 C3 1.356(7) . ?
N4 C30 1.451(7) . ?
N4 C4 1.484(6) . ?
N5 C7 1.370(7) . ?
N5 C5 1.450(8) . ?
N5 C10 1.480(7) . ?
N6 C7 1.373(8) . ?
N6 C8 1.458(7) . ?
N6 C11 1.459(7) . ?
N7 C9 1.369(8) . ?
N7 C12 1.467(7) . ?
N7 C8 1.478(7) . ?
N8 C9 1.368(7) . ?
N8 C6 1.472(8) . ?
N8 C10 1.475(7) . ?
N9 C13 1.358(8) . ?
N9 C11 1.479(7) . ?
N9 C16 1.496(7) . ?
N10 C13 1.371(7) . ?
N10 C14 1.465(7) . ?
N10 C17 1.470(8) . ?
N11 C15 1.378(7) . ?
N11 C14 1.466(7) . ?
N11 C18 1.467(7) . ?
N12 C15 1.380(8) . ?
N12 C12 1.443(7) . ?
N12 C16 1.481(8) . ?
N13 C19 1.377(8) . ?
N13 C17 1.449(9) . ?
N13 C22 1.474(7) . ?
N14 C19 1.345(8) . ?
N14 C23 1.477(8) . ?
N14 C20 1.484(7) . ?
N15 C21 1.364(8) . ?
N15 C24 1.454(9) . ?
N15 C20 1.487(7) . ?
N16 C21 1.381(9) . ?
N16 C18 1.446(9) . ?
N16 C22 1.492(7) . ?
N17 C25 1.375(7) . ?
N17 C28 1.459(8) . ?
N17 C23 1.460(8) . ?
N18 C25 1.389(7) . ?
N18 C29 1.459(7) . ?
N18 C26 1.473(8) . ?
N19 C27 1.373(7) . ?
N19 C26 1.466(8) . ?
N19 C30 1.466(7) . ?
N20 C27 1.373(8) . ?
N20 C28 1.467(7) . ?
N20 C24 1.472(7) . ?
C2 C31 1.545(9) . ?
C4 C31 1.530(8) . ?
C8 C36 1.550(8) . ?
C10 C36 1.526(10) . ?
C14 C41 1.541(10) . ?
C16 C41 1.509(9) . ?
C20 C46 1.535(9) . ?
C22 C46 1.513(9) . ?
C26 C51 1.488(9) . ?
C28 C51 1.527(10) . ?
C31 C35 1.549(8) . ?
C31 C32 1.549(7) . ?
C32 C33 1.501(10) . ?
C33 C34 1.525(13) . ?
C34 C35 1.542(10) . ?
C36 C40 1.539(9) . ?
C36 C37 1.551(9) . ?
C37 C38 1.479(13) . ?
C38 C39 1.579(15) . ?
C39 C40 1.523(12) . ?
C41 C45 1.510(10) . ?
C41 C42 1.545(9) . ?
C42 C43 1.553(11) . ?
C43 C44 1.490(12) . ?
C44 C45 1.511(11) . ?
C46 C50 1.547(8) . ?
C46 C47 1.561(8) . ?
C47 C48 1.536(9) . ?
C48 C49 1.513(12) . ?
C49 C50 1.501(9) . ?
C51 C52 1.518(10) . ?
C51 C55 1.564(11) . ?
C52 C53 1.415(15) . ?
C53 C54 1.460(14) . ?
C54 C55 1.522(11) . ?

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
O11 Ca1 O3 90.46(17) . . ?
O11 Ca1 O9 94.52(17) . . ?
O3 Ca1 O9 144.46(15) . . ?
O11 Ca1 O7 92.89(16) . . ?
O3 Ca1 O7 143.00(17) . . ?
O9 Ca1 O7 71.92(15) . . ?
O11 Ca1 O1 89.57(16) . . ?
O3 Ca1 O1 73.45(15) . . ?
O9 Ca1 O1 71.43(14) . . ?
O7 Ca1 O1 143.35(16) . . ?
O11 Ca1 O5 90.60(16) . . ?
O3 Ca1 O5 71.16(14) . . ?
O9 Ca1 O5 143.73(13) . . ?
O7 Ca1 O5 71.97(15) . . ?
O1 Ca1 O5 144.61(14) . . ?
O11 Ca1 Cl1 178.23(14) . . ?
O3 Ca1 Cl1 87.78(10) . . ?
O9 Ca1 Cl1 86.85(10) . . ?
O7 Ca1 Cl1 88.60(10) . . ?
O1 Ca1 Cl1 89.80(9) . . ?
O5 Ca1 Cl1 88.95(9) . . ?
O12 Ca2 O6 97.66(16) . . ?
O12 Ca2 O4 93.44(15) . . ?
O6 Ca2 O4 73.48(14) . . ?
O12 Ca2 O10 86.69(16) . . ?
O6 Ca2 O10 142.76(14) . . ?
O4 Ca2 O10 143.46(14) . . ?
O12 Ca2 O2 87.26(15) . . ?
O6 Ca2 O2 144.03(15) . . ?
O4 Ca2 O2 70.67(14) . . ?
O10 Ca2 O2 72.84(14) . . ?
O12 Ca2 O8 91.62(15) . . ?
O6 Ca2 O8 71.22(15) . . ?
O4 Ca2 O8 144.70(15) . . ?
O10 Ca2 O8 71.70(15) . . ?
O2 Ca2 O8 144.53(16) . . ?
O12 Ca2 Cl1 173.73(14) . . ?
O6 Ca2 Cl1 88.48(10) . . ?
O4 Ca2 Cl1 89.54(10) . . ?
O10 Ca2 Cl1 87.63(10) . . ?
O2 Ca2 Cl1 88.52(9) . . ?
O8 Ca2 Cl1 89.13(10) . . ?
Ca2 Cl1 Ca1 178.36(7) . . ?
C1 O1 Ca1 127.6(3) . . ?
C3 O2 Ca2 129.0(3) . . ?
C7 O3 Ca1 133.6(3) . . ?
C9 O4 Ca2 131.0(3) . . ?
C13 O5 Ca1 130.3(4) . . ?
C15 O6 Ca2 132.0(4) . . ?
C19 O7 Ca1 127.4(3) . . ?
C21 O8 Ca2 127.8(3) . . ?
C25 O9 Ca1 133.1(4) . . ?
C27 O10 Ca2 131.0(4) . . ?
C1 N1 C29 119.7(5) . . ?
C1 N1 C4 122.6(4) . . ?
C29 N1 C4 117.6(5) . . ?
C1 N2 C2 122.4(5) . . ?
C1 N2 C5 119.2(4) . . ?
C2 N2 C5 118.4(4) . . ?
C3 N3 C6 118.9(4) . . ?
C3 N3 C2 122.2(5) . . ?
C6 N3 C2 118.7(4) . . ?
C3 N4 C30 118.2(4) . . ?
C3 N4 C4 123.7(5) . . ?
C30 N4 C4 118.0(4) . . ?
C7 N5 C5 119.7(5) . . ?
C7 N5 C10 121.6(5) . . ?
C5 N5 C10 118.6(5) . . ?
C7 N6 C8 122.8(5) . . ?
C7 N6 C11 118.6(5) . . ?
C8 N6 C11 118.6(5) . . ?
C9 N7 C12 119.8(5) . . ?
C9 N7 C8 122.3(5) . . ?
C12 N7 C8 117.7(5) . . ?
C9 N8 C6 119.5(4) . . ?
C9 N8 C10 122.7(5) . . ?
C6 N8 C10 117.4(4) . . ?
C13 N9 C11 118.2(5) . . ?
C13 N9 C16 123.6(4) . . ?
C11 N9 C16 118.1(5) . . ?
C13 N10 C14 121.7(5) . . ?
C13 N10 C17 118.4(5) . . ?
C14 N10 C17 119.6(4) . . ?
C15 N11 C14 122.6(5) . . ?
C15 N11 C18 118.6(4) . . ?
C14 N11 C18 118.8(4) . . ?
C15 N12 C12 118.6(5) . . ?
C15 N12 C16 122.5(5) . . ?
C12 N12 C16 118.8(5) . . ?
C19 N13 C17 120.0(5) . . ?
C19 N13 C22 121.0(5) . . ?
C17 N13 C22 118.7(5) . . ?
C19 N14 C23 121.6(5) . . ?
C19 N14 C20 121.3(5) . . ?
C23 N14 C20 117.0(5) . . ?
C21 N15 C24 118.7(5) . . ?
C21 N15 C20 122.2(5) . . ?
C24 N15 C20 119.0(5) . . ?
C21 N16 C18 120.6(5) . . ?
C21 N16 C22 121.3(5) . . ?
C18 N16 C22 118.1(5) . . ?
C25 N17 C28 123.5(5) . . ?
C25 N17 C23 117.2(5) . . ?
C28 N17 C23 119.1(5) . . ?
C25 N18 C29 117.8(5) . . ?
C25 N18 C26 122.8(5) . . ?
C29 N18 C26 119.4(5) . . ?
C27 N19 C26 121.8(5) . . ?
C27 N19 C30 117.7(5) . . ?
C26 N19 C30 120.4(4) . . ?
C27 N20 C28 122.0(5) . . ?
C27 N20 C24 118.9(5) . . ?
C28 N20 C24 119.1(5) . . ?
O1 C1 N1 122.1(5) . . ?
O1 C1 N2 121.2(6) . . ?
N1 C1 N2 116.6(5) . . ?
N2 C2 N3 111.8(4) . . ?
N2 C2 C31 110.6(4) . . ?
N3 C2 C31 109.1(4) . . ?
O2 C3 N4 122.2(5) . . ?
O2 C3 N3 120.9(5) . . ?
N4 C3 N3 116.9(4) . . ?
N4 C4 N1 109.9(4) . . ?
N4 C4 C31 109.9(4) . . ?
N1 C4 C31 108.7(4) . . ?
N5 C5 N2 115.7(4) . . ?
N3 C6 N8 118.3(4) . . ?
O3 C7 N5 121.0(6) . . ?
O3 C7 N6 121.5(5) . . ?
N5 C7 N6 117.4(5) . . ?
N6 C8 N7 112.1(5) . . ?
N6 C8 C36 109.6(5) . . ?
N7 C8 C36 108.6(5) . . ?
O4 C9 N8 121.6(5) . . ?
O4 C9 N7 121.5(5) . . ?
N8 C9 N7 116.9(5) . . ?
N8 C10 N5 112.3(4) . . ?
N8 C10 C36 108.5(5) . . ?
N5 C10 C36 110.1(5) . . ?
N6 C11 N9 114.6(4) . . ?
N12 C12 N7 115.6(5) . . ?
O5 C13 N9 122.3(5) . . ?
O5 C13 N10 121.0(5) . . ?
N9 C13 N10 116.6(5) . . ?
N10 C14 N11 111.2(5) . . ?
N10 C14 C41 111.3(5) . . ?
N11 C14 C41 109.0(5) . . ?
O6 C15 N11 121.7(5) . . ?
O6 C15 N12 121.9(5) . . ?
N11 C15 N12 116.4(5) . . ?
N12 C16 N9 108.9(5) . . ?
N12 C16 C41 109.6(5) . . ?
N9 C16 C41 109.9(5) . . ?
N13 C17 N10 115.0(5) . . ?
N16 C18 N11 114.9(4) . . ?
O7 C19 N14 120.7(6) . . ?
O7 C19 N13 119.9(6) . . ?
N14 C19 N13 119.3(5) . . ?
N14 C20 N15 111.5(4) . . ?
N14 C20 C46 109.7(5) . . ?
N15 C20 C46 109.1(5) . . ?
O8 C21 N15 122.1(6) . . ?
O8 C21 N16 120.1(6) . . ?
N15 C21 N16 117.6(5) . . ?
N13 C22 N16 110.1(4) . . ?
N13 C22 C46 111.0(5) . . ?
N16 C22 C46 109.6(5) . . ?
N17 C23 N14 115.4(5) . . ?
N15 C24 N20 115.3(5) . . ?
O9 C25 N17 123.3(5) . . ?
O9 C25 N18 122.0(5) . . ?
N17 C25 N18 114.6(5) . . ?
N19 C26 N18 110.2(5) . . ?
N19 C26 C51 110.7(5) . . ?
N18 C26 C51 109.8(5) . . ?
O10 C27 N19 122.1(5) . . ?
O10 C27 N20 120.8(5) . . ?
N19 C27 N20 117.0(5) . . ?
N17 C28 N20 112.8(5) . . ?
N17 C28 C51 108.5(5) . . ?
N20 C28 C51 109.4(5) . . ?
N18 C29 N1 114.6(4) . . ?
N4 C30 N19 115.0(5) . . ?
C4 C31 C2 102.9(4) . . ?
C4 C31 C35 112.3(5) . . ?
C2 C31 C35 112.2(5) . . ?
C4 C31 C32 111.7(5) . . ?
C2 C31 C32 112.9(5) . . ?
C35 C31 C32 105.1(4) . . ?
C33 C32 C31 105.8(5) . . ?
C32 C33 C34 105.7(6) . . ?
C33 C34 C35 100.8(7) . . ?
C34 C35 C31 105.0(5) . . ?
C10 C36 C40 115.0(6) . . ?
C10 C36 C8 102.9(5) . . ?
C40 C36 C8 111.7(5) . . ?
C10 C36 C37 113.7(6) . . ?
C40 C36 C37 103.9(5) . . ?
C8 C36 C37 109.9(5) . . ?
C38 C37 C36 105.7(6) . . ?
C37 C38 C39 106.2(7) . . ?
C40 C39 C38 106.5(7) . . ?
C39 C40 C36 105.9(6) . . ?
C16 C41 C45 113.7(5) . . ?
C16 C41 C14 103.1(6) . . ?
C45 C41 C14 114.0(5) . . ?
C16 C41 C42 111.6(5) . . ?
C45 C41 C42 103.3(6) . . ?
C14 C41 C42 111.5(5) . . ?
C41 C42 C43 105.2(6) . . ?
C44 C43 C42 106.5(7) . . ?
C43 C44 C45 107.0(7) . . ?
C41 C45 C44 104.9(6) . . ?
C22 C46 C20 103.5(5) . . ?
C22 C46 C50 112.2(5) . . ?
C20 C46 C50 114.0(6) . . ?
C22 C46 C47 111.8(6) . . ?
C20 C46 C47 110.5(5) . . ?
C50 C46 C47 105.0(5) . . ?
C48 C47 C46 105.0(5) . . ?
C49 C48 C47 103.4(6) . . ?
C50 C49 C48 105.7(6) . . ?
C49 C50 C46 106.9(5) . . ?
C26 C51 C52 113.3(6) . . ?
C26 C51 C28 103.9(5) . . ?
C52 C51 C28 113.5(6) . . ?
C26 C51 C55 112.2(6) . . ?
C52 C51 C55 103.6(6) . . ?
C28 C51 C55 110.6(6) . . ?
C53 C52 C51 109.4(8) . . ?
C52 C53 C54 111.4(10) . . ?
C53 C54 C55 106.9(9) . . ?
C54 C55 C51 106.1(7) . . ?

_refine_diff_density_max         1.797
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.189

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_mo_40926aa
_database_code_depnum_ccdc_archive 'CCDC 1505409'
_audit_update_record             
;
2017-06-14 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H76 Ca2 Cl4 N16 O18'
_chemical_formula_weight         1339.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.6660(10)
_cell_length_b                   20.7418(16)
_cell_length_c                   11.6720(9)
_cell_angle_alpha                90
_cell_angle_beta                 111.6460(10)
_cell_angle_gamma                90
_cell_volume                     2850.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    7362
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.44

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.473
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17930
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.964
_diffrn_reflns_theta_max         26.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5836
_reflns_number_gt                4898
_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_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0892P)²+1.9593P] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5836
_refine_ls_number_parameters     454
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ca1 Ca 0.17521(4) 0.49477(2) 0.75795(4) 0.01792(14) Uani 1 1 d . . . . .
Cl1 Cl 0.42946(5) 0.42264(3) 0.58834(6) 0.03507(18) Uani 1 1 d . . . . .
Cl2 Cl 0.02087(6) 0.67977(3) 0.51027(6) 0.03703(19) Uani 1 1 d . . . . .
N1 N 0.26203(15) 0.43809(8) 1.13764(16) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.13739(15) 0.35886(8) 1.01882(16) 0.0172(4) Uani 1 1 d . . . . .
N3 N -0.04572(14) 0.36216(8) 0.84607(16) 0.0165(4) Uani 1 1 d . . . . .
N4 N -0.16638(15) 0.44132(9) 0.72337(16) 0.0180(4) Uani 1 1 d . . . . .
N5 N -0.16175(15) 0.55996(9) 0.71883(16) 0.0177(4) Uani 1 1 d . . . . .
N6 N -0.03516(15) 0.63735(9) 0.84044(16) 0.0173(4) Uani 1 1 d . . . . .
N7 N 0.14839(15) 0.63632(8) 1.01333(16) 0.0169(4) Uani 1 1 d . . . . .
N8 N 0.26829(15) 0.55631(8) 1.13438(16) 0.0168(4) Uani 1 1 d . . . . .
O1 O 0.22391(14) 0.42882(8) 0.93294(14) 0.0232(3) Uani 1 1 d . . . . .
O2 O 0.01463(13) 0.43118(8) 0.73228(15) 0.0231(3) Uani 1 1 d . . . . .
O3 O 0.02129(13) 0.56298(8) 0.73256(15) 0.0235(3) Uani 1 1 d . . . . .
O4 O 0.23837(14) 0.56619(8) 0.93079(14) 0.0226(3) Uani 1 1 d . . . . .
O5 O 0.37952(15) 0.47546(11) 0.81668(18) 0.0370(4) Uani 1 1 d . . . . .
H5A H 0.410(4) 0.457(2) 0.755(4) 0.092(14) Uiso 1 1 d . . . . .
H5B H 0.396(5) 0.439(3) 0.872(6) 0.139 Uiso 1 1 d . U . . .
O6 O 0.1749(2) 0.41893(12) 0.6074(2) 0.0495(6) Uani 1 1 d . . . . .
H6A H 0.231(4) 0.413(2) 0.579(4) 0.077(13) Uiso 1 1 d . . . . .
H6B H 0.129(5) 0.392(3) 0.575(5) 0.108(19) Uiso 1 1 d . . . . .
O7 O 0.21282(19) 0.57774(10) 0.6384(2) 0.0417(5) Uani 1 1 d D . . . .
H7A H 0.164(3) 0.6031(18) 0.593(3) 0.079(14) Uiso 1 1 d D . . . .
H7B H 0.2705(19) 0.5827(17) 0.625(3) 0.057(11) Uiso 1 1 d D . . . .
C1 C 0.20803(17) 0.40964(10) 1.02521(19) 0.0173(4) Uani 1 1 d . . . . .
C2 C 0.12514(18) 0.33174(10) 1.12909(19) 0.0172(4) Uani 1 1 d . . . . .
H2 H 0.1073 0.2853 1.1148 0.021 Uiso 1 1 calc R U . . .
C3 C 0.23849(17) 0.33879(10) 1.23815(19) 0.0184(4) Uani 1 1 d . . . . .
C4 C 0.25449(17) 0.41178(10) 1.25128(19) 0.0171(4) Uani 1 1 d . . . . .
H4 H 0.3270 0.4207 1.3203 0.021 Uiso 1 1 calc R U . . .
C5 C 0.06736(17) 0.33327(10) 0.89780(19) 0.0168(4) Uani 1 1 d . . . . .
H5C H 0.1067 0.3405 0.8406 0.020 Uiso 1 1 calc R U . . .
H5D H 0.0592 0.2866 0.9048 0.020 Uiso 1 1 calc R U . . .
C6 C -0.06205(18) 0.41261(10) 0.76582(19) 0.0168(4) Uani 1 1 d . . . . .
C7 C -0.26089(17) 0.41583(10) 0.75329(19) 0.0172(4) Uani 1 1 d . . . . .
H7 H -0.3325 0.4256 0.6837 0.021 Uiso 1 1 calc R U . . .
C8 C -0.25001(17) 0.34275(10) 0.76740(19) 0.0181(4) Uani 1 1 d . . . . .
C9 C -0.13757(17) 0.33447(10) 0.87708(19) 0.0166(4) Uani 1 1 d . . . . .
H9 H -0.1228 0.2878 0.8926 0.020 Uiso 1 1 calc R U . . .
C10 C -0.18168(19) 0.49964(9) 0.6487(2) 0.0177(4) Uani 1 1 d . . . . .
H10A H -0.2594 0.5001 0.5875 0.021 Uiso 1 1 calc R U . . .
H10B H -0.1298 0.4978 0.6039 0.021 Uiso 1 1 calc R U . . .
C11 C -0.05511(18) 0.58549(10) 0.76300(19) 0.0174(4) Uani 1 1 d . . . . .
C12 C 0.08028(17) 0.66297(10) 0.89226(19) 0.0169(4) Uani 1 1 d . . . . .
H12A H 0.0763 0.7099 0.8995 0.020 Uiso 1 1 calc R U . . .
H12B H 0.1188 0.6539 0.8350 0.020 Uiso 1 1 calc R U . . .
C13 C 0.21864(17) 0.58508(10) 1.02165(19) 0.0171(4) Uani 1 1 d . . . . .
C14 C 0.33009(18) 0.49596(9) 1.1437(2) 0.0177(4) Uani 1 1 d . . . . .
H14A H 0.3955 0.4957 1.2217 0.021 Uiso 1 1 calc R U . . .
H14B H 0.3592 0.4943 1.0767 0.021 Uiso 1 1 calc R U . . .
C15 C 0.33685(19) 0.30477(11) 1.2131(2) 0.0240(5) Uani 0.603(14) 1 d . . P A 1
H15A H 0.3073 0.2802 1.1360 0.029 Uiso 0.603(14) 1 calc R U P A 1
H15B H 0.3914 0.3366 1.2063 0.029 Uiso 0.603(14) 1 calc R U P A 1
C16 C 0.3932(5) 0.2602(4) 1.3203(6) 0.0361(18) Uani 0.603(14) 1 d . U P A 1
H16A H 0.4534 0.2825 1.3868 0.043 Uiso 0.603(14) 1 calc R U P A 1
H16B H 0.4257 0.2225 1.2948 0.043 Uiso 0.603(14) 1 calc R U P A 1
C17 C 0.2949(10) 0.2406(6) 1.3612(12) 0.033(2) Uani 0.603(14) 1 d . U P A 1
H17A H 0.2444 0.2092 1.3044 0.040 Uiso 0.603(14) 1 calc R U P A 1
H17B H 0.3233 0.2228 1.4449 0.040 Uiso 0.603(14) 1 calc R U P A 1
C18 C 0.2354(2) 0.30565(11) 1.3557(2) 0.0237(5) Uani 0.603(14) 1 d . . P A 1
H18A H 0.2758 0.3316 1.4291 0.028 Uiso 0.603(14) 1 calc R U P A 1
H18B H 0.1570 0.2993 1.3500 0.028 Uiso 0.603(14) 1 calc R U P A 1
C19 C -0.2482(2) 0.30837(11) 0.6505(2) 0.0236(5) Uani 0.626(16) 1 d . . P B 1
H19A H -0.2929 0.3323 0.5759 0.028 Uiso 0.626(16) 1 calc R U P B 1
H19B H -0.1703 0.3037 0.6533 0.028 Uiso 0.626(16) 1 calc R U P B 1
C20 C -0.3014(8) 0.2425(4) 0.6534(9) 0.0298(17) Uani 0.626(16) 1 d . U P B 1
H20A H -0.3290 0.2222 0.5718 0.036 Uiso 0.626(16) 1 calc R U P B 1
H20B H -0.2471 0.2135 0.7126 0.036 Uiso 0.626(16) 1 calc R U P B 1
C21 C -0.3994(6) 0.2596(3) 0.6940(7) 0.0344(16) Uani 0.626(16) 1 d . U P B 1
H21A H -0.4641 0.2767 0.6250 0.041 Uiso 0.626(16) 1 calc R U P B 1
H21B H -0.4243 0.2218 0.7278 0.041 Uiso 0.626(16) 1 calc R U P B 1
C22 C -0.34954(19) 0.31067(11) 0.7927(2) 0.0230(5) Uani 0.626(16) 1 d . . P B 1
H22A H -0.3221 0.2909 0.8747 0.028 Uiso 0.626(16) 1 calc R U P B 1
H22B H -0.4073 0.3429 0.7890 0.028 Uiso 0.626(16) 1 calc R U P B 1
C15' C 0.33685(19) 0.30477(11) 1.2131(2) 0.0240(5) Uani 0.397(14) 1 d . . P A 2
H15C H 0.3209 0.3018 1.1245 0.029 Uiso 0.397(14) 1 calc R U P A 2
H15D H 0.4088 0.3277 1.2530 0.029 Uiso 0.397(14) 1 calc R U P A 2
C16' C 0.3404(11) 0.2390(4) 1.2687(12) 0.045(3) Uani 0.397(14) 1 d . U P A 2
H16C H 0.2808 0.2112 1.2136 0.055 Uiso 0.397(14) 1 calc R U P A 2
H16D H 0.4144 0.2185 1.2861 0.055 Uiso 0.397(14) 1 calc R U P A 2
C17' C 0.3207(17) 0.2524(11) 1.385(2) 0.043(4) Uani 0.397(14) 1 d . U P A 2
H17C H 0.2915 0.2139 1.4125 0.052 Uiso 0.397(14) 1 calc R U P A 2
H17D H 0.3916 0.2655 1.4512 0.052 Uiso 0.397(14) 1 calc R U P A 2
C18' C 0.2354(2) 0.30565(11) 1.3557(2) 0.0237(5) Uani 0.397(14) 1 d . . P A 2
H18C H 0.2550 0.3365 1.4240 0.028 Uiso 0.397(14) 1 calc R U P A 2
H18D H 0.1595 0.2884 1.3409 0.028 Uiso 0.397(14) 1 calc R U P A 2
C19' C -0.2482(2) 0.30837(11) 0.6505(2) 0.0236(5) Uani 0.374(16) 1 d . . P B 2
H19C H -0.2702 0.3384 0.5807 0.028 Uiso 0.374(16) 1 calc R U P B 2
H19D H -0.1719 0.2920 0.6644 0.028 Uiso 0.374(16) 1 calc R U P B 2
C20' C -0.3305(14) 0.2545(10) 0.6248(16) 0.052(5) Uani 0.374(16) 1 d . U P B 2
H20C H -0.2992 0.2156 0.6015 0.062 Uiso 0.374(16) 1 calc R U P B 2
H20D H -0.4015 0.2658 0.5575 0.062 Uiso 0.374(16) 1 calc R U P B 2
C21' C -0.3511(13) 0.2433(5) 0.7422(14) 0.044(3) Uani 0.374(16) 1 d . U P B 2
H21C H -0.2911 0.2165 0.7997 0.053 Uiso 0.374(16) 1 calc R U P B 2
H21D H -0.4247 0.2224 0.7255 0.053 Uiso 0.374(16) 1 calc R U P B 2
C22' C -0.34954(19) 0.31067(11) 0.7927(2) 0.0230(5) Uani 0.374(16) 1 d . . P B
2
H22C H -0.3353 0.3097 0.8811 0.028 Uiso 0.374(16) 1 calc R U P B 2
H22D H -0.4213 0.3332 0.7494 0.028 Uiso 0.374(16) 1 calc R U P B 2
O8 O 0.5102(2) 0.40822(14) 0.0373(3) 0.0639(7) Uani 1 1 d D . . . .
H8A H 0.573(3) 0.397(2) 0.032(4) 0.096 Uiso 1 1 d D U . . .
H8B H 0.522(4) 0.407(2) 0.114(2) 0.096 Uiso 1 1 d D U . . .
O9 O 0.42663(19) 0.57545(11) 0.5935(2) 0.0422(5) Uani 1 1 d D . . . .
H9A H 0.457(3) 0.5885(14) 0.553(3) 0.044(10) Uiso 1 1 d D . . . .
H9B H 0.425(3) 0.5365(9) 0.594(3) 0.061(12) Uiso 1 1 d 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 2.3376(16) . ?
Ca1 O1 2.3439(16) . ?
Ca1 O2 2.3487(16) . ?
Ca1 O6 2.358(2) . ?
Ca1 O7 2.3722(19) . ?
Ca1 O4 2.3903(16) . ?
Ca1 O5 2.4532(19) . ?
N1 C1 1.370(3) . ?
N1 C14 1.464(3) . ?
N1 C4 1.470(3) . ?
N2 C1 1.366(3) . ?
N2 C5 1.463(3) . ?
N2 C2 1.464(3) . ?
N3 C6 1.368(3) . ?
N3 C9 1.458(3) . ?
N3 C5 1.462(3) . ?
N4 C6 1.365(3) . ?
N4 C10 1.461(3) . ?
N4 C7 1.464(3) . ?
N5 C11 1.363(3) . ?
N5 C10 1.465(3) . ?
N5 C4 1.465(3) 3_567 ?
N6 C11 1.367(3) . ?
N6 C12 1.461(3) . ?
N6 C2 1.461(3) 3_567 ?
N7 C13 1.366(3) . ?
N7 C12 1.465(3) . ?
N7 C9 1.467(3) 3_567 ?
N8 C13 1.368(3) . ?
N8 C14 1.459(3) . ?
N8 C7 1.467(3) 3_567 ?
O1 C1 1.232(3) . ?
O2 C6 1.235(3) . ?
O3 C11 1.239(3) . ?
O4 C13 1.239(3) . ?
O5 H5A 1.01(5) . ?
O5 H5B 0.97(7) . ?
O6 H6A 0.89(5) . ?
O6 H6B 0.80(6) . ?
O7 H7A 0.836(18) . ?
O7 H7B 0.810(18) . ?
C2 N6 1.461(3) 3_567 ?
C2 C3 1.535(3) . ?
C2 H2 0.9900 . ?
C3 C4 1.528(3) . ?
C3 C18 1.548(3) . ?
C3 C15 1.551(3) . ?
C4 N5 1.466(3) 3_567 ?
C4 H4 0.9900 . ?
C5 H5C 0.9800 . ?
C5 H5D 0.9800 . ?
C7 N8 1.467(3) 3_567 ?
C7 C8 1.525(3) . ?
C7 H7 0.9900 . ?
C8 C9 1.533(3) . ?
C8 C22 1.547(3) . ?
C8 C19 1.548(3) . ?
C9 N7 1.467(3) 3_567 ?
C9 H9 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.507(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 C17 1.543(12) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.535(12) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.530(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 C21 1.525(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C21 C22 1.520(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C16' C17' 1.50(3) . ?
C16' H16C 0.9800 . ?
C16' H16D 0.9800 . ?
C17' H17C 0.9800 . ?
C17' H17D 0.9800 . ?
C20' C21' 1.50(2) . ?
C20' H20C 0.9800 . ?
C20' H20D 0.9800 . ?
C21' H21C 0.9800 . ?
C21' H21D 0.9800 . ?
O8 H8A 0.857(19) . ?
O8 H8B 0.847(19) . ?
O9 H9A 0.765(17) . ?
O9 H9B 0.809(18) . ?

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 O1 113.75(6) . . ?
O3 Ca1 O2 71.41(6) . . ?
O1 Ca1 O2 73.78(6) . . ?
O3 Ca1 O6 122.51(8) . . ?
O1 Ca1 O6 100.82(8) . . ?
O2 Ca1 O6 76.53(7) . . ?
O3 Ca1 O7 79.95(7) . . ?
O1 Ca1 O7 152.96(7) . . ?
O2 Ca1 O7 133.21(7) . . ?
O6 Ca1 O7 89.48(9) . . ?
O3 Ca1 O4 74.68(5) . . ?
O1 Ca1 O4 74.20(6) . . ?
O2 Ca1 O4 117.40(6) . . ?
O6 Ca1 O4 161.92(7) . . ?
O7 Ca1 O4 88.26(7) . . ?
O3 Ca1 O5 151.49(7) . . ?
O1 Ca1 O5 75.51(7) . . ?
O2 Ca1 O5 135.93(7) . . ?
O6 Ca1 O5 79.09(8) . . ?
O7 Ca1 O5 82.11(8) . . ?
O4 Ca1 O5 82.83(6) . . ?
C1 N1 C14 118.44(17) . . ?
C1 N1 C4 121.94(17) . . ?
C14 N1 C4 119.61(17) . . ?
C1 N2 C5 118.96(17) . . ?
C1 N2 C2 121.86(17) . . ?
C5 N2 C2 119.09(17) . . ?
C6 N3 C9 122.57(17) . . ?
C6 N3 C5 118.28(17) . . ?
C9 N3 C5 119.08(17) . . ?
C6 N4 C10 118.37(18) . . ?
C6 N4 C7 121.55(18) . . ?
C10 N4 C7 120.07(17) . . ?
C11 N5 C10 119.06(18) . . ?
C11 N5 C4 121.61(17) . 3_567 ?
C10 N5 C4 119.12(17) . 3_567 ?
C11 N6 C12 118.20(17) . . ?
C11 N6 C2 122.38(17) . 3_567 ?
C12 N6 C2 119.41(17) . 3_567 ?
C13 N7 C12 119.88(17) . . ?
C13 N7 C9 121.81(17) . 3_567 ?
C12 N7 C9 118.30(16) . 3_567 ?
C13 N8 C14 119.28(17) . . ?
C13 N8 C7 121.96(17) . 3_567 ?
C14 N8 C7 118.75(17) . 3_567 ?
C1 O1 Ca1 151.00(15) . . ?
C6 O2 Ca1 151.63(15) . . ?
C11 O3 Ca1 153.52(15) . . ?
C13 O4 Ca1 143.87(15) . . ?
Ca1 O5 H5A 120(3) . . ?
Ca1 O5 H5B 105(4) . . ?
H5A O5 H5B 98(4) . . ?
Ca1 O6 H6A 126(3) . . ?
Ca1 O6 H6B 129(4) . . ?
H6A O6 H6B 106(4) . . ?
Ca1 O7 H7A 124(3) . . ?
Ca1 O7 H7B 127(2) . . ?
H7A O7 H7B 108(3) . . ?
O1 C1 N2 121.06(19) . . ?
O1 C1 N1 120.91(19) . . ?
N2 C1 N1 118.03(18) . . ?
N6 C2 N2 112.98(16) 3_567 . ?
N6 C2 C3 109.35(17) 3_567 . ?
N2 C2 C3 108.81(17) . . ?
N6 C2 H2 108.5 3_567 . ?
N2 C2 H2 108.5 . . ?
C3 C2 H2 108.5 . . ?
C4 C3 C2 103.09(16) . . ?
C4 C3 C18 113.38(18) . . ?
C2 C3 C18 111.80(18) . . ?
C4 C3 C15 112.57(18) . . ?
C2 C3 C15 111.79(18) . . ?
C18 C3 C15 104.46(17) . . ?
N5 C4 N1 113.01(16) 3_567 . ?
N5 C4 C3 109.40(17) 3_567 . ?
N1 C4 C3 109.14(17) . . ?
N5 C4 H4 108.4 3_567 . ?
N1 C4 H4 108.4 . . ?
C3 C4 H4 108.4 . . ?
N3 C5 N2 113.76(16) . . ?
N3 C5 H5C 108.8 . . ?
N2 C5 H5C 108.8 . . ?
N3 C5 H5D 108.8 . . ?
N2 C5 H5D 108.8 . . ?
H5C C5 H5D 107.7 . . ?
O2 C6 N4 121.20(19) . . ?
O2 C6 N3 121.17(19) . . ?
N4 C6 N3 117.63(18) . . ?
N4 C7 N8 113.48(16) . 3_567 ?
N4 C7 C8 109.60(17) . . ?
N8 C7 C8 109.14(17) 3_567 . ?
N4 C7 H7 108.2 . . ?
N8 C7 H7 108.2 3_567 . ?
C8 C7 H7 108.2 . . ?
C7 C8 C9 102.74(16) . . ?
C7 C8 C22 113.61(18) . . ?
C9 C8 C22 111.34(17) . . ?
C7 C8 C19 113.13(18) . . ?
C9 C8 C19 111.92(17) . . ?
C22 C8 C19 104.36(17) . . ?
N3 C9 N7 113.17(16) . 3_567 ?
N3 C9 C8 109.21(17) . . ?
N7 C9 C8 108.97(16) 3_567 . ?
N3 C9 H9 108.5 . . ?
N7 C9 H9 108.5 3_567 . ?
C8 C9 H9 108.5 . . ?
N4 C10 N5 114.59(18) . . ?
N4 C10 H10A 108.6 . . ?
N5 C10 H10A 108.6 . . ?
N4 C10 H10B 108.6 . . ?
N5 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
O3 C11 N5 121.01(19) . . ?
O3 C11 N6 120.85(19) . . ?
N5 C11 N6 118.13(18) . . ?
N6 C12 N7 113.92(16) . . ?
N6 C12 H12A 108.8 . . ?
N7 C12 H12A 108.8 . . ?
N6 C12 H12B 108.8 . . ?
N7 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O4 C13 N7 121.10(19) . . ?
O4 C13 N8 121.25(19) . . ?
N7 C13 N8 117.63(18) . . ?
N8 C14 N1 114.18(18) . . ?
N8 C14 H14A 108.7 . . ?
N1 C14 H14A 108.7 . . ?
N8 C14 H14B 108.7 . . ?
N1 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C16 C15 C3 106.8(2) . . ?
C16 C15 H15A 110.4 . . ?
C3 C15 H15A 110.4 . . ?
C16 C15 H15B 110.4 . . ?
C3 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 C17 103.3(6) . . ?
C15 C16 H16A 111.1 . . ?
C17 C16 H16A 111.1 . . ?
C15 C16 H16B 111.1 . . ?
C17 C16 H16B 111.1 . . ?
H16A C16 H16B 109.1 . . ?
C18 C17 C16 101.2(8) . . ?
C18 C17 H17A 111.5 . . ?
C16 C17 H17A 111.5 . . ?
C18 C17 H17B 111.5 . . ?
C16 C17 H17B 111.5 . . ?
H17A C17 H17B 109.3 . . ?
C17 C18 C3 104.8(5) . . ?
C17 C18 H18A 110.8 . . ?
C3 C18 H18A 110.8 . . ?
C17 C18 H18B 110.8 . . ?
C3 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C20 C19 C8 104.0(4) . . ?
C20 C19 H19A 111.0 . . ?
C8 C19 H19A 111.0 . . ?
C20 C19 H19B 111.0 . . ?
C8 C19 H19B 111.0 . . ?
H19A C19 H19B 109.0 . . ?
C21 C20 C19 102.4(6) . . ?
C21 C20 H20A 111.3 . . ?
C19 C20 H20A 111.3 . . ?
C21 C20 H20B 111.3 . . ?
C19 C20 H20B 111.3 . . ?
H20A C20 H20B 109.2 . . ?
C22 C21 C20 103.8(5) . . ?
C22 C21 H21A 111.0 . . ?
C20 C21 H21A 111.0 . . ?
C22 C21 H21B 111.0 . . ?
C20 C21 H21B 111.0 . . ?
H21A C21 H21B 109.0 . . ?
C21 C22 C8 107.2(2) . . ?
C21 C22 H22A 110.3 . . ?
C8 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
C8 C22 H22B 110.3 . . ?
H22A C22 H22B 108.5 . . ?
C17' C16' H16C 111.0 . . ?
C17' C16' H16D 111.0 . . ?
H16C C16' H16D 109.0 . . ?
C16' C17' H17C 110.6 . . ?
C16' C17' H17D 110.6 . . ?
H17C C17' H17D 108.7 . . ?
C21' C20' H20C 110.5 . . ?
C21' C20' H20D 110.5 . . ?
H20C C20' H20D 108.7 . . ?
C20' C21' H21C 111.1 . . ?
C20' C21' H21D 111.1 . . ?
H21C C21' H21D 109.1 . . ?
H8A O8 H8B 105(3) . . ?
H9A O9 H9B 112(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 N2 89.3(3) . . . . ?
Ca1 O1 C1 N1 -91.7(3) . . . . ?
C5 N2 C1 O1 -9.0(3) . . . . ?
C2 N2 C1 O1 174.51(19) . . . . ?
C5 N2 C1 N1 171.94(17) . . . . ?
C2 N2 C1 N1 -4.6(3) . . . . ?
C14 N1 C1 O1 6.1(3) . . . . ?
C4 N1 C1 O1 -173.14(19) . . . . ?
C14 N1 C1 N2 -174.78(18) . . . . ?
C4 N1 C1 N2 5.9(3) . . . . ?
C1 N2 C2 N6 89.7(2) . . . 3_567 ?
C5 N2 C2 N6 -86.8(2) . . . 3_567 ?
C1 N2 C2 C3 -31.9(2) . . . . ?
C5 N2 C2 C3 151.58(17) . . . . ?
N6 C2 C3 C4 -60.8(2) 3_567 . . . ?
N2 C2 C3 C4 63.0(2) . . . . ?
N6 C2 C3 C18 61.3(2) 3_567 . . . ?
N2 C2 C3 C18 -174.88(17) . . . . ?
N6 C2 C3 C15 178.01(17) 3_567 . . . ?
N2 C2 C3 C15 -58.2(2) . . . . ?
C1 N1 C4 N5 -92.4(2) . . . 3_567 ?
C14 N1 C4 N5 88.3(2) . . . 3_567 ?
C1 N1 C4 C3 29.6(3) . . . . ?
C14 N1 C4 C3 -149.71(18) . . . . ?
C2 C3 C4 N5 62.3(2) . . . 3_567 ?
C18 C3 C4 N5 -58.7(2) . . . 3_567 ?
C15 C3 C4 N5 -177.04(16) . . . 3_567 ?
C2 C3 C4 N1 -61.8(2) . . . . ?
C18 C3 C4 N1 177.16(16) . . . . ?
C15 C3 C4 N1 58.8(2) . . . . ?
C6 N3 C5 N2 95.5(2) . . . . ?
C9 N3 C5 N2 -87.3(2) . . . . ?
C1 N2 C5 N3 -92.4(2) . . . . ?
C2 N2 C5 N3 84.2(2) . . . . ?
Ca1 O2 C6 N4 93.2(3) . . . . ?
Ca1 O2 C6 N3 -87.4(3) . . . . ?
C10 N4 C6 O2 -7.3(3) . . . . ?
C7 N4 C6 O2 174.10(19) . . . . ?
C10 N4 C6 N3 173.27(17) . . . . ?
C7 N4 C6 N3 -5.3(3) . . . . ?
C9 N3 C6 O2 -173.10(18) . . . . ?
C5 N3 C6 O2 4.0(3) . . . . ?
C9 N3 C6 N4 6.3(3) . . . . ?
C5 N3 C6 N4 -176.59(17) . . . . ?
C6 N4 C7 N8 90.8(2) . . . 3_567 ?
C10 N4 C7 N8 -87.8(2) . . . 3_567 ?
C6 N4 C7 C8 -31.5(3) . . . . ?
C10 N4 C7 C8 149.95(18) . . . . ?
N4 C7 C8 C9 62.5(2) . . . . ?
N8 C7 C8 C9 -62.3(2) 3_567 . . . ?
N4 C7 C8 C22 -177.06(16) . . . . ?
N8 C7 C8 C22 58.1(2) 3_567 . . . ?
N4 C7 C8 C19 -58.3(2) . . . . ?
N8 C7 C8 C19 176.86(16) 3_567 . . . ?
C6 N3 C9 N7 -92.2(2) . . . 3_567 ?
C5 N3 C9 N7 90.7(2) . . . 3_567 ?
C6 N3 C9 C8 29.3(3) . . . . ?
C5 N3 C9 C8 -147.69(17) . . . . ?
C7 C8 C9 N3 -61.3(2) . . . . ?
C22 C8 C9 N3 176.75(17) . . . . ?
C19 C8 C9 N3 60.4(2) . . . . ?
C7 C8 C9 N7 62.8(2) . . . 3_567 ?
C22 C8 C9 N7 -59.2(2) . . . 3_567 ?
C19 C8 C9 N7 -175.54(17) . . . 3_567 ?
C6 N4 C10 N5 -92.0(2) . . . . ?
C7 N4 C10 N5 86.7(2) . . . . ?
C11 N5 C10 N4 89.9(2) . . . . ?
C4 N5 C10 N4 -84.8(2) 3_567 . . . ?
Ca1 O3 C11 N5 -92.3(4) . . . . ?
Ca1 O3 C11 N6 88.7(4) . . . . ?
C10 N5 C11 O3 8.7(3) . . . . ?
C4 N5 C11 O3 -176.65(19) 3_567 . . . ?
C10 N5 C11 N6 -172.29(17) . . . . ?
C4 N5 C11 N6 2.3(3) 3_567 . . . ?
C12 N6 C11 O3 -3.7(3) . . . . ?
C2 N6 C11 O3 175.22(19) 3_567 . . . ?
C12 N6 C11 N5 177.29(17) . . . . ?
C2 N6 C11 N5 -3.8(3) 3_567 . . . ?
C11 N6 C12 N7 -93.5(2) . . . . ?
C2 N6 C12 N7 87.6(2) 3_567 . . . ?
C13 N7 C12 N6 95.1(2) . . . . ?
C9 N7 C12 N6 -84.1(2) 3_567 . . . ?
Ca1 O4 C13 N7 -89.8(3) . . . . ?
Ca1 O4 C13 N8 91.6(3) . . . . ?
C12 N7 C13 O4 10.3(3) . . . . ?
C9 N7 C13 O4 -170.51(18) 3_567 . . . ?
C12 N7 C13 N8 -171.14(17) . . . . ?
C9 N7 C13 N8 8.1(3) 3_567 . . . ?
C14 N8 C13 O4 -10.4(3) . . . . ?
C7 N8 C13 O4 169.91(19) 3_567 . . . ?
C14 N8 C13 N7 171.01(18) . . . . ?
C7 N8 C13 N7 -8.7(3) 3_567 . . . ?
C13 N8 C14 N1 -94.1(2) . . . . ?
C7 N8 C14 N1 85.6(2) 3_567 . . . ?
C1 N1 C14 N8 92.8(2) . . . . ?
C4 N1 C14 N8 -87.9(2) . . . . ?
C4 C3 C15 C16 117.5(4) . . . . ?
C2 C3 C15 C16 -127.0(4) . . . . ?
C18 C3 C15 C16 -5.9(4) . . . . ?
C3 C15 C16 C17 30.7(8) . . . . ?
C15 C16 C17 C18 -43.4(9) . . . . ?
C16 C17 C18 C3 39.9(8) . . . . ?
C4 C3 C18 C17 -144.3(5) . . . . ?
C2 C3 C18 C17 99.7(5) . . . . ?
C15 C3 C18 C17 -21.4(5) . . . . ?
C7 C8 C19 C20 -149.9(4) . . . . ?
C9 C8 C19 C20 94.6(4) . . . . ?
C22 C8 C19 C20 -25.9(4) . . . . ?
C8 C19 C20 C21 41.3(7) . . . . ?
C19 C20 C21 C22 -40.5(8) . . . . ?
C20 C21 C22 C8 24.5(7) . . . . ?
C7 C8 C22 C21 124.6(4) . . . . ?
C9 C8 C22 C21 -120.0(4) . . . . ?
C19 C8 C22 C21 0.9(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9B Cl1 0.809(18) 2.363(19) 3.171(3) 176(3) .
O9 H9A Cl1 0.765(17) 2.56(2) 3.268(2) 154(3) 3_666
O8 H8A O4 0.857(19) 2.39(4) 3.112(3) 142(4) 3_666
C9 H9 Cl2 0.99 2.63 3.574(2) 160.6 2_546
C5 H5D Cl2 0.98 2.77 3.664(2) 152.2 2_546
C2 H2 Cl2 0.99 2.79 3.713(2) 154.5 2_546
O7 H7B O9 0.810(18) 2.144(19) 2.942(3) 169(3) .
O7 H7A Cl2 0.836(18) 2.33(2) 3.153(2) 167(4) .
O6 H6B Cl2 0.80(6) 2.32(6) 3.117(2) 172(5) 3_566
O6 H6A Cl1 0.89(5) 2.48(5) 3.313(2) 154(4) .
O5 H5B O8 0.97(7) 2.04(7) 2.859(3) 141(5) 1_556
O5 H5A Cl1 1.01(5) 2.17(5) 3.154(2) 165(4) .

_refine_diff_density_max         1.031
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.098

_shelxl_version_number           2013-2

