#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:29:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179020 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/18/4121812.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4121812
loop_
_publ_author_name
'Howe, Ethan N. W.'
'Bhadbhade, Mohan'
'Thordarson, Pall'
_publ_section_title
;
 Cooperativity and complexity in the binding of anions and cations to a
 tetratopic ion-pair host.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7505
_journal_page_last               7516
_journal_paper_doi               10.1021/ja503383e
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C18 H30 Ca1 N2 O7, 2(Cl O4)'
_chemical_formula_sum            'C18 H30 Ca Cl2 N2 O15'
_chemical_formula_weight         625.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                101.24(3)
_cell_angle_beta                 92.31(3)
_cell_angle_gamma                110.51(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2180(16)
_cell_length_b                   9.6910(19)
_cell_length_c                   18.377(4)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     1335.1(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and OLEX-2 (Dolomanov et al., 2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'ADSC Quantum 210r'
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16914
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.276
_diffrn_source                   'Synchrotron BM'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       plates
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0904P)²+6.7778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3556
_reflns_number_total             4367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja503383e_si_003.cif
_cod_data_source_block           Host+2[Ca(ClO4)2].4H2O
_cod_depositor_comments
'Adding full bibliography for 4121812--4121813.cif.'
_cod_original_cell_volume        1335.0(5)
_cod_database_code               4121812
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.80564(13) 0.16640(11) 0.77089(5) 0.0228(3) Uani 1 1 d . . . . .
O1W O 0.7404(6) 0.3851(4) 0.7826(2) 0.0385(10) Uani 1 1 d . . . . .
H1A H 0.6319 0.3683 0.7930 0.058 Uiso 1 1 d R U . . .
H1B H 0.7510 0.4179 0.7406 0.058 Uiso 1 1 d R U . . .
O2W O 0.8648(6) -0.0515(5) 0.7775(2) 0.0476(11) Uani 1 1 d . . . . .
H1D H 0.9404 -0.0365 0.8183 0.071 Uiso 1 1 d R U . . .
H1C H 0.9134 -0.0821 0.7371 0.071 Uiso 1 1 d R U . . .
O1 O 0.5399(5) 0.0145(4) 0.70504(19) 0.0343(9) Uani 1 1 d . . . . .
O2 O 0.1273(5) -0.1851(4) 0.34645(18) 0.0301(8) Uani 1 1 d . . . . .
O3 O 0.6025(5) 0.1022(4) 0.86564(17) 0.0318(9) Uani 1 1 d . . . . .
O5 O 1.1220(5) 0.3089(6) 0.7828(2) 0.0489(12) Uani 1 1 d . . . . .
N1 N 0.2663(6) -0.1435(5) 0.7058(2) 0.0290(10) Uani 1 1 d . . . . .
H1N H 0.1597 -0.1819 0.6851 0.035 Uiso 1 1 calc R U . . .
N2 N -0.0480(6) -0.3233(4) 0.4169(2) 0.0262(9) Uani 1 1 d . . . . .
H2N H -0.0809 -0.3277 0.4605 0.031 Uiso 1 1 calc R U . . .
C6 C 0.1900(7) -0.0902(6) 0.4768(3) 0.0263(11) Uani 1 1 d . . . . .
C1 C 0.2167(7) -0.1261(5) 0.5449(3) 0.0249(11) Uani 1 1 d . . . . .
H1 H 0.1545 -0.2220 0.5523 0.030 Uiso 1 1 calc R U . . .
C2 C 0.3376(7) -0.0173(5) 0.6025(3) 0.0256(11) Uani 1 1 d . . . . .
C3 C 0.4274(7) 0.1268(6) 0.5915(3) 0.0299(12) Uani 1 1 d . . . . .
H3 H 0.5101 0.1980 0.6292 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3955(8) 0.1654(6) 0.5255(3) 0.0323(12) Uani 1 1 d . . . . .
H4 H 0.4517 0.2635 0.5196 0.039 Uiso 1 1 calc R U . . .
C5 C 0.2786(8) 0.0565(6) 0.4679(3) 0.0294(12) Uani 1 1 d . . . . .
H5 H 0.2591 0.0815 0.4228 0.035 Uiso 1 1 calc R U . . .
C7 C 0.3884(7) -0.0493(5) 0.6746(3) 0.0264(11) Uani 1 1 d . . . . .
C8 C 0.0855(7) -0.2043(6) 0.4089(3) 0.0272(11) Uani 1 1 d . . . . .
C9 C 0.3123(8) -0.1824(6) 0.7754(3) 0.0373(14) Uani 1 1 d . . . . .
H9A H 0.4308 -0.1814 0.7762 0.045 Uiso 1 1 calc R U . . .
H9B H 0.2351 -0.2845 0.7753 0.045 Uiso 1 1 calc R U . . .
C10 C 0.3002(8) -0.0767(7) 0.8464(3) 0.0401(14) Uani 1 1 d . . . . .
H10A H 0.1816 -0.0781 0.8456 0.048 Uiso 1 1 calc R U . . .
H10B H 0.3229 -0.1155 0.8890 0.048 Uiso 1 1 calc R U . . .
C11 C 0.4246(8) 0.0849(6) 0.8573(3) 0.0356(13) Uani 1 1 d . . . . .
H11A H 0.4026 0.1239 0.8147 0.043 Uiso 1 1 calc R U . . .
H11B H 0.4008 0.1450 0.9014 0.043 Uiso 1 1 calc R U . . .
C12 C 0.6839(9) 0.1444(9) 0.9419(3) 0.057(2) Uani 0.5 1 d . . P A 1
H12A H 0.5967 0.1513 0.9750 0.069 Uiso 0.5 1 calc R U P A 1
H12B H 0.7218 0.0647 0.9513 0.069 Uiso 0.5 1 calc R U P A 1
C13 C 0.8289(15) 0.2825(13) 0.9601(5) 0.032(2) Uani 0.5 1 d . . P A 1
H13A H 0.8915 0.2932 1.0080 0.039 Uiso 0.5 1 calc R U P A 1
H13B H 0.7900 0.3669 0.9631 0.039 Uiso 0.5 1 calc R U P A 1
O4 O 0.9432(5) 0.2800(4) 0.90063(18) 0.0321(9) Uani 0.5 1 d . . P A 1
C14 C 1.1276(14) 0.3107(13) 0.9073(5) 0.032(3) Uani 0.5 1 d . . P A 1
H14A H 1.1477 0.2163 0.8981 0.039 Uiso 0.5 1 calc R U P A 1
H14B H 1.1798 0.3665 0.9576 0.039 Uiso 0.5 1 calc R U P A 1
C15 C 1.2082(9) 0.3979(7) 0.8542(4) 0.0442(15) Uani 0.5 1 d . . P A 1
H15A H 1.1926 0.4943 0.8637 0.053 Uiso 0.5 1 calc R U P A 1
H15B H 1.3324 0.4164 0.8571 0.053 Uiso 0.5 1 calc R U P A 1
C12' C 0.6839(9) 0.1444(9) 0.9419(3) 0.057(2) Uani 0.5 1 d . . P A 2
H12C H 0.6588 0.2302 0.9684 0.069 Uiso 0.5 1 calc R U P A 2
H12D H 0.6320 0.0611 0.9659 0.069 Uiso 0.5 1 calc R U P A 2
C13' C 0.8547(15) 0.1798(13) 0.9480(5) 0.032(3) Uani 0.5 1 d . . P A 2
H13C H 0.8790 0.0875 0.9354 0.038 Uiso 0.5 1 calc R U P A 2
H13D H 0.9025 0.2279 0.9996 0.038 Uiso 0.5 1 calc R U P A 2
O4' O 0.9432(5) 0.2800(4) 0.90063(18) 0.0321(9) Uani 0.5 1 d . . P A 2
C14' C 1.0828(15) 0.4299(12) 0.9116(6) 0.034(2) Uani 0.5 1 d . . P A 2
H14C H 1.1411 0.4644 0.9623 0.040 Uiso 0.5 1 calc R U P A 2
H14D H 1.0376 0.5042 0.9001 0.040 Uiso 0.5 1 calc R U P A 2
C15' C 1.2082(9) 0.3979(7) 0.8542(4) 0.0442(15) Uani 0.5 1 d . . P A 2
H15C H 1.2902 0.4938 0.8478 0.053 Uiso 0.5 1 calc R U P A 2
H15D H 1.2751 0.3468 0.8749 0.053 Uiso 0.5 1 calc R U P A 2
C16 C 1.2378(8) 0.2958(7) 0.7271(3) 0.0394(14) Uani 1 1 d . . . . .
H16A H 1.1802 0.2027 0.6898 0.047 Uiso 1 1 calc R U . . .
H16B H 1.3420 0.2896 0.7506 0.047 Uiso 1 1 calc R U . . .
C17 C 1.2914(7) 0.4275(6) 0.6884(3) 0.0317(12) Uani 1 1 d . . . . .
H17A H 1.3531 0.5198 0.7256 0.038 Uiso 1 1 calc R U . . .
H17B H 1.3725 0.4134 0.6534 0.038 Uiso 1 1 calc R U . . .
C18 C 1.1408(7) 0.4472(6) 0.6467(3) 0.0288(11) Uani 1 1 d . . . . .
H18A H 1.0580 0.4584 0.6814 0.035 Uiso 1 1 calc R U . . .
H18B H 1.1858 0.5400 0.6291 0.035 Uiso 1 1 calc R U . . .
Cl1A Cl 0.6962(4) 0.7041(3) 0.90527(15) 0.0422(7) Uiso 0.7 1 d D U P B 1
O1A O 0.6207(9) 0.6797(8) 0.8277(4) 0.0609(19) Uiso 0.7 1 d D U P B 1
O2A O 0.6944(7) 0.5598(5) 0.9138(3) 0.0668(14) Uiso 0.7 1 d D U P B 1
O3A O 0.8619(9) 0.8165(8) 0.9153(5) 0.096(3) Uiso 0.7 1 d D U P B 1
O4A O 0.5777(11) 0.7459(10) 0.9514(5) 0.100(3) Uiso 0.7 1 d D U P B 1
Cl1' Cl 0.6615(12) 0.6882(8) 0.9191(5) 0.065(3) Uiso 0.3 1 d D . P C 2
O1A' O 0.502(2) 0.669(2) 0.9444(13) 0.122(10) Uiso 0.3 1 d D . P C 2
O2A' O 0.6944(7) 0.5598(5) 0.9138(3) 0.0668(14) Uiso 0.3 1 d D . P C 2
O3A' O 0.659(3) 0.725(2) 0.8519(9) 0.158(15) Uiso 0.3 1 d D . P C 2
O4A' O 0.786(3) 0.804(3) 0.9691(11) 0.118(9) Uiso 0.3 1 d D . P C 2
Cl1B Cl 0.75913(18) 0.59713(14) 0.61306(7) 0.0321(3) Uani 1 1 d . . . . .
O1B O 0.7210(6) 0.4726(5) 0.6479(2) 0.0405(10) Uani 1 1 d . . . . .
O2B O 0.6067(7) 0.6287(6) 0.6006(3) 0.0713(17) Uani 1 1 d . . . . .
O3B O 0.8303(8) 0.5596(5) 0.5453(2) 0.0665(16) Uani 1 1 d . . . . .
O4B O 0.8905(6) 0.7288(5) 0.6595(3) 0.0596(14) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 Ca1 O1 80.89(13) 2_656 .
O2 Ca1 O1W 89.11(14) 2_656 .
O1 Ca1 O1W 93.32(16) . .
O2 Ca1 O2W 99.19(15) 2_656 .
O1 Ca1 O2W 88.87(17) . .
O1W Ca1 O2W 171.66(14) . .
O2 Ca1 O5 73.64(13) 2_656 .
O1 Ca1 O5 153.75(14) . .
O1W Ca1 O5 92.56(17) . .
O2W Ca1 O5 88.99(18) . .
O2 Ca1 O4 138.33(14) 2_656 .
O1 Ca1 O4 140.36(14) . .
O1W Ca1 O4 83.85(14) . .
O2W Ca1 O4 89.32(15) . .
O5 Ca1 O4 65.76(13) . .
O2 Ca1 O3 154.21(14) 2_656 .
O1 Ca1 O3 74.22(13) . .
O1W Ca1 O3 85.72(14) . .
O2W Ca1 O3 87.13(15) . .
O5 Ca1 O3 131.77(13) . .
O4 Ca1 O3 66.13(12) . .
O2 Ca1 H1A 98.4 2_656 .
O1 Ca1 H1A 80.5 . .
O1W Ca1 H1A 17.3 . .
O2W Ca1 H1A 157.7 . .
O5 Ca1 H1A 109.1 . .
O4 Ca1 H1A 86.6 . .
O3 Ca1 H1A 71.2 . .
O2 Ca1 H1B 71.8 2_656 .
O1 Ca1 H1B 89.6 . .
O1W Ca1 H1B 17.3 . .
O2W Ca1 H1B 171.0 . .
O5 Ca1 H1B 88.5 . .
O4 Ca1 H1B 97.5 . .
O3 Ca1 H1B 100.9 . .
H1A Ca1 H1B 29.8 . .
Ca1 O1W H1A 111.1 . .
Ca1 O1W H1B 111.1 . .
H1A O1W H1B 107.7 . .
Ca1 O2W H1D 112.3 . .
Ca1 O2W H1C 111.7 . .
H1D O2W H1C 106.7 . .
C7 O1 Ca1 170.0(4) . .
C8 O2 Ca1 176.2(3) . 2_656
C11 O3 C12 115.1(4) . .
C11 O3 Ca1 124.8(3) . .
C12 O3 Ca1 115.4(3) . .
C15 O5 C16 114.5(5) . .
C15 O5 Ca1 118.3(4) . .
C16 O5 Ca1 126.5(4) . .
C7 N1 C9 120.6(5) . .
C7 N1 H1N 119.7 . .
C9 N1 H1N 119.7 . .
C8 N2 C18 121.4(4) . 2_656
C8 N2 H2N 119.3 . .
C18 N2 H2N 119.3 2_656 .
C1 C6 C5 119.4(5) . .
C1 C6 C8 123.5(4) . .
C5 C6 C8 116.8(4) . .
C6 C1 C2 119.8(4) . .
C6 C1 H1 120.1 . .
C2 C1 H1 120.1 . .
C3 C2 C1 119.7(4) . .
C3 C2 C7 116.4(5) . .
C1 C2 C7 123.7(4) . .
C4 C3 C2 120.8(5) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C3 C4 C5 119.4(5) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
C4 C5 C6 120.8(5) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
O1 C7 N1 121.3(5) . .
O1 C7 C2 119.7(4) . .
N1 C7 C2 118.9(5) . .
O2 C8 N2 121.9(5) . .
O2 C8 C6 118.9(5) . .
N2 C8 C6 119.2(4) . .
N1 C9 C10 114.3(5) . .
N1 C9 H9A 108.7 . .
C10 C9 H9A 108.7 . .
N1 C9 H9B 108.7 . .
C10 C9 H9B 108.7 . .
H9A C9 H9B 107.6 . .
C11 C10 C9 114.7(4) . .
C11 C10 H10A 108.6 . .
C9 C10 H10A 108.6 . .
C11 C10 H10B 108.6 . .
C9 C10 H10B 108.6 . .
H10A C10 H10B 107.6 . .
O3 C11 C10 113.7(5) . .
O3 C11 H11A 108.8 . .
C10 C11 H11A 108.8 . .
O3 C11 H11B 108.8 . .
C10 C11 H11B 108.8 . .
H11A C11 H11B 107.7 . .
C13 C12 O3 114.8(6) . .
C13 C12 H12A 108.6 . .
O3 C12 H12A 108.6 . .
C13 C12 H12B 108.6 . .
O3 C12 H12B 108.6 . .
H12A C12 H12B 107.5 . .
C12 C13 O4 107.3(8) . .
C12 C13 H13A 110.3 . .
O4 C13 H13A 110.3 . .
C12 C13 H13B 110.3 . .
O4 C13 H13B 110.3 . .
H13A C13 H13B 108.5 . .
C14 O4 C13 128.9(6) . .
C14 O4 Ca1 111.9(4) . .
C13 O4 Ca1 118.3(5) . .
O4 C14 C15 110.1(8) . .
O4 C14 H14A 109.6 . .
C15 C14 H14A 109.6 . .
O4 C14 H14B 109.6 . .
C15 C14 H14B 109.6 . .
H14A C14 H14B 108.2 . .
O5 C15 C14 105.6(6) . .
O5 C15 H15A 110.6 . .
C14 C15 H15A 110.6 . .
O5 C15 H15B 110.6 . .
C14 C15 H15B 110.6 . .
H15A C15 H15B 108.8 . .
H13C C13' H13D 107.7 . .
H14C C14' H14D 109.3 . .
O5 C16 C17 113.1(5) . .
O5 C16 H16A 109.0 . .
C17 C16 H16A 109.0 . .
O5 C16 H16B 109.0 . .
C17 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C18 C17 C16 114.7(5) . .
C18 C17 H17A 108.6 . .
C16 C17 H17A 108.6 . .
C18 C17 H17B 108.6 . .
C16 C17 H17B 108.6 . .
H17A C17 H17B 107.6 . .
N2 C18 C17 114.6(4) 2_656 .
N2 C18 H18A 108.6 2_656 .
C17 C18 H18A 108.6 . .
N2 C18 H18B 108.6 2_656 .
C17 C18 H18B 108.6 . .
H18A C18 H18B 107.6 . .
O3A Cl1A O4A 113.2(4) . .
O3A Cl1A O2A 114.7(4) . .
O4A Cl1A O2A 109.1(4) . .
O3A Cl1A O1A 107.7(4) . .
O4A Cl1A O1A 105.8(4) . .
O2A Cl1A O1A 105.6(3) . .
O3A' Cl1' O4A' 109.5(7) . .
O3A' Cl1' O1A' 108.9(6) . .
O4A' Cl1' O1A' 108.0(7) . .
O2B Cl1B O1B 109.9(3) . .
O2B Cl1B O4B 108.9(3) . .
O1B Cl1B O4B 110.4(3) . .
O2B Cl1B O3B 112.7(4) . .
O1B Cl1B O3B 107.5(3) . .
O4B Cl1B O3B 107.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.273(3) 2_656
Ca1 O1 2.290(4) .
Ca1 O1W 2.335(4) .
Ca1 O2W 2.351(4) .
Ca1 O5 2.457(4) .
Ca1 O4 2.462(4) .
Ca1 O3 2.477(4) .
Ca1 H1A 2.7801 .
Ca1 H1B 2.7796 .
O1W H1A 0.8852 .
O1W H1B 0.8852 .
O2W H1D 0.9080 .
O2W H1C 0.9064 .
O1 C7 1.231(6) .
O2 C8 1.240(6) .
O2 Ca1 2.272(3) 2_656
O3 C11 1.411(7) .
O3 C12 1.445(6) .
O5 C15 1.421(8) .
O5 C16 1.443(7) .
N1 C7 1.333(7) .
N1 C9 1.474(6) .
N1 H1N 0.8600 .
N2 C8 1.322(7) .
N2 C18 1.459(6) 2_656
N2 H2N 0.8600 .
C6 C1 1.392(7) .
C6 C5 1.398(7) .
C6 C8 1.494(7) .
C1 C2 1.401(7) .
C1 H1 0.9300 .
C2 C3 1.391(7) .
C2 C7 1.494(7) .
C3 C4 1.379(7) .
C3 H3 0.9300 .
C4 C5 1.389(8) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C9 C10 1.524(9) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.509(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.414(13) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 O4 1.472(11) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
O4 C14 1.433(12) .
C14 C15 1.445(12) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C13' H13C 0.9700 .
C13' H13D 0.9700 .
C14' H14C 0.9700 .
C14' H14D 0.9700 .
C16 C17 1.520(8) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 C18 1.517(8) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 N2 1.459(6) 2_656
C18 H18A 0.9700 .
C18 H18B 0.9700 .
Cl1A O3A 1.392(7) .
Cl1A O4A 1.428(7) .
Cl1A O2A 1.432(5) .
Cl1A O1A 1.472(6) .
Cl1' O3A' 1.353(12) .
Cl1' O4A' 1.366(12) .
Cl1' O1A' 1.368(12) .
Cl1B O2B 1.410(5) .
Cl1B O1B 1.421(4) .
Cl1B O4B 1.434(4) .
Cl1B O3B 1.434(5) .
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_4
C5 C6 C1 C2 -2.9(8) . .
C8 C6 C1 C2 170.3(5) . .
C6 C1 C2 C3 1.3(8) . .
C6 C1 C2 C7 -173.7(5) . .
C1 C2 C3 C4 1.8(8) . .
C7 C2 C3 C4 177.2(5) . .
C2 C3 C4 C5 -3.3(8) . .
C3 C4 C5 C6 1.6(8) . .
C1 C6 C5 C4 1.5(8) . .
C8 C6 C5 C4 -172.2(5) . .
Ca1 O1 C7 N1 -92(2) . .
Ca1 O1 C7 C2 86.0(19) . .
C9 N1 C7 O1 -4.4(8) . .
C9 N1 C7 C2 177.7(5) . .
C3 C2 C7 O1 -30.8(7) . .
C1 C2 C7 O1 144.4(5) . .
C3 C2 C7 N1 147.2(5) . .
C1 C2 C7 N1 -37.7(8) . .
C18 N2 C8 O2 7.3(8) 2_656 .
C18 N2 C8 C6 -172.3(5) 2_656 .
C1 C6 C8 O2 -147.9(5) . .
C5 C6 C8 O2 25.4(8) . .
C1 C6 C8 N2 31.7(8) . .
C5 C6 C8 N2 -154.9(5) . .
C7 N1 C9 C10 89.6(6) . .
N1 C9 C10 C11 -63.1(7) . .
C12 O3 C11 C10 -96.8(6) . .
Ca1 O3 C11 C10 108.7(4) . .
C9 C10 C11 O3 -63.3(6) . .
C11 O3 C12 C13 -120.4(8) . .
Ca1 O3 C12 C13 36.6(10) . .
O3 C12 C13 O4 -47.8(11) . .
C12 C13 O4 C14 -129.3(9) . .
C12 C13 O4 Ca1 38.4(10) . .
C13 O4 C14 C15 -139.3(8) . .
Ca1 O4 C14 C15 52.3(8) . .
C16 O5 C15 C14 -133.0(7) . .
Ca1 O5 C15 C14 38.3(8) . .
O4 C14 C15 O5 -58.4(9) . .
C15 O5 C16 C17 -84.5(6) . .
Ca1 O5 C16 C17 104.9(5) . .
O5 C16 C17 C18 -60.7(7) . .
C16 C17 C18 N2 -65.0(6) . 2_656
