#------------------------------------------------------------------------------
#$Date: 2017-05-23 03:58:20 +0300 (Tue, 23 May 2017) $
#$Revision: 196887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/01/7120172.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_7120172
loop_
_publ_author_name
'Lavendomme, Roy'
'Ajami, Daniela'
'Moerkerke, Steven'
'Wouters, Johan'
'Rissanen, Kari'
'Luhmer, Michel'
'Jabin, Ivan'
_publ_section_title
;
 Encapsulation and solid state sequestration of gases by
 calix[6]arene-based molecular containers
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03078A
_journal_year                    2017
_chemical_formula_moiety         '4(C2H4Cl2), C96H144N6O12'
_chemical_formula_sum            'C104 H138 Cl8 N6 O12'
_chemical_formula_weight         1947.8
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-06
_audit_creation_method           SHELXL-2014/8
_audit_update_record
;
2017-04-18 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                97.571(4)
_cell_angle_beta                 109.693(5)
_cell_angle_gamma                114.255(5)
_cell_formula_units_Z            1
_cell_length_a                   13.7784(9)
_cell_length_b                   14.3195(7)
_cell_length_c                   16.9560(8)
_cell_measurement_reflns_used    3116
_cell_measurement_temperature    149.8
_cell_measurement_theta_max      62.3786
_cell_measurement_theta_min      3.5638
_cell_volume                     2725.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.8
_diffrn_detector_area_resol_mean 5.1856
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -28.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -1.1041   38.0000    0.0000 103

#__ type_ start__ end____ width___ exp.time_
  2 omega -117.00  -13.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   77.0000   30.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega -171.00    5.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000    0.0000    0.0000 176

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00  114.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257  -61.0000  120.0000 104

#__ type_ start__ end____ width___ exp.time_
  5 omega   18.00   97.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       83.9257 -126.0000  120.0000 79
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0113631000
_diffrn_orient_matrix_UB_12      -0.0468253000
_diffrn_orient_matrix_UB_13      0.0773391000
_diffrn_orient_matrix_UB_21      0.0932832000
_diffrn_orient_matrix_UB_22      0.1136652000
_diffrn_orient_matrix_UB_23      0.0652387000
_diffrn_orient_matrix_UB_31      -0.0983582000
_diffrn_orient_matrix_UB_32      0.0185291000
_diffrn_orient_matrix_UB_33      0.0099567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.855
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9569
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        62.470
_diffrn_reflns_theta_max         62.470
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.35
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.649
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.611
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1316
_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          0.3837
_refine_ls_wR_factor_ref         0.4171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5252
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc03078a2.cif
_cod_data_source_block           C2H4Cl2_4
_cod_database_code               7120172
_shelx_shelxl_version_number     2016/4
_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.
;
_reflns_odcompleteness_completeness 90.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
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
O21 O 0.8161(3) 0.3372(3) 0.6373(3) 0.0372(10) Uani 1 1 d . U . . .
O41 O 0.4861(4) 0.2209(3) 0.3270(2) 0.0390(10) Uani 1 1 d . U . . .
O42 O 0.5247(4) 0.3139(4) 0.2327(3) 0.0518(12) Uani 1 1 d . U . . .
O1 O 0.5551(4) 0.1490(4) 0.7893(3) 0.0543(13) Uani 1 1 d . U . . .
O2 O 0.6699(5) 0.2513(5) 0.9340(3) 0.0613(14) Uani 1 1 d . U . . .
O22 O 0.9253(5) 0.5137(4) 0.7152(5) 0.087(2) Uani 1 1 d . U . . .
N1 N 0.4822(6) 0.2143(5) 0.8644(4) 0.0619(17) Uani 1 1 d . U . . .
H1 H 0.4219 0.1811 0.8138 0.074 Uiso 1 1 calc R U . . .
N21 N 1.0081(4) 0.4146(4) 0.6877(4) 0.0468(13) Uani 1 1 d . U . . .
H21 H 0.9904 0.3491 0.6655 0.056 Uiso 1 1 calc R U . . .
N41 N 0.3719(5) 0.2883(5) 0.2689(3) 0.0473(14) Uani 1 1 d . U . . .
H41 H 0.3473 0.2708 0.3078 0.057 Uiso 1 1 calc R U . . .
C41 C 0.5822(5) 0.2034(4) 0.3400(3) 0.0300(12) Uani 1 1 d . U . . .
C42 C 0.6871(5) 0.2700(5) 0.4166(4) 0.0347(13) Uani 1 1 d . U . . .
C24 C 0.7100(5) 0.3368(4) 0.6223(4) 0.0344(13) Uani 1 1 d . U . . .
C23 C 0.6655(5) 0.3213(4) 0.6843(4) 0.0353(14) Uani 1 1 d . U . . .
C25 C 0.6472(5) 0.3459(4) 0.5418(4) 0.0348(13) Uani 1 1 d . U . . .
C31 C 0.7005(5) 0.3690(5) 0.4774(4) 0.0370(14) Uani 1 1 d . U . . .
H31A H 0.7840 0.4205 0.5105 0.044 Uiso 1 1 calc R U . . .
H31B H 0.6644 0.4030 0.4407 0.044 Uiso 1 1 calc R U . . .
C46 C 0.5704(5) 0.1190(5) 0.2806(4) 0.0396(14) Uani 1 1 d . U . . .
C52 C 0.4648(5) 0.2787(5) 0.2706(4) 0.0378(14) Uani 1 1 d . U . . .
C43 C 0.7784(5) 0.2482(5) 0.4325(4) 0.0388(14) Uani 1 1 d . U . . .
H43 H 0.8480 0.2917 0.4836 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4850(6) 0.3125(5) 0.5826(4) 0.0404(14) Uani 1 1 d . U . . .
C32 C 0.9201(6) 0.4323(5) 0.6833(4) 0.0424(15) Uani 1 1 d . U . . .
C26 C 0.5378(6) 0.3351(5) 0.5250(4) 0.0391(14) Uani 1 1 d . U . . .
H26 H 0.4967 0.3432 0.4727 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7396(5) 0.3213(5) 0.7747(3) 0.0364(14) Uani 1 1 d . U . . .
H11A H 0.8205 0.3774 0.7946 0.044 Uiso 1 1 calc R U . . .
H11B H 0.7112 0.3404 0.8160 0.044 Uiso 1 1 calc R U . . .
C45 C 0.6662(6) 0.1020(5) 0.2995(4) 0.0445(16) Uani 1 1 d . U . . .
H45 H 0.6602 0.0463 0.2596 0.053 Uiso 1 1 calc R U . . .
C44 C 0.7725(6) 0.1649(5) 0.3763(4) 0.0424(15) Uani 1 1 d . U . . .
C51 C 0.4579(6) 0.0491(5) 0.1966(4) 0.0450(16) Uani 1 1 d . U . . .
H51A H 0.4757 0.0129 0.1555 0.054 Uiso 1 1 calc R U . . .
H51B H 0.4317 0.0956 0.1702 0.054 Uiso 1 1 calc R U . . .
C22 C 0.5540(5) 0.3087(5) 0.6632(4) 0.0370(14) Uani 1 1 d . U . . .
H22 H 0.5233 0.2972 0.7043 0.044 Uiso 1 1 calc R U . . .
C1 C 0.8297(6) 0.0998(6) 0.7773(5) 0.0530(18) Uani 1 1 d . U . . .
C4 C 0.6436(6) 0.1343(5) 0.7870(4) 0.0423(16) Uani 1 1 d . U . . .
C27 C 0.3615(6) 0.2955(5) 0.5567(4) 0.0470(16) Uani 1 1 d . U . . .
C7 C 0.9380(6) 0.0916(6) 0.7798(5) 0.0477(16) Uani 1 1 d . U . . .
C53 C 0.3079(6) 0.3274(6) 0.2039(4) 0.0497(17) Uani 1 1 d . U . . .
C47 C 0.8771(7) 0.1432(7) 0.3947(5) 0.0574(19) Uani 1 1 d . U . . .
C33 C 1.1331(6) 0.4960(6) 0.7268(5) 0.0526(18) Uani 1 1 d . U . . .
C13 C 0.4679(7) 0.2690(7) 0.9351(5) 0.062(2) Uani 1 1 d . U . . .
C28 C 0.3221(6) 0.2758(7) 0.6318(5) 0.061(2) Uani 1 1 d . U . . .
H28A H 0.2434 0.2653 0.6135 0.092 Uiso 1 1 calc R U . . .
H28B H 0.3237 0.2128 0.6442 0.092 Uiso 1 1 calc R U . . .
H28C H 0.3749 0.3372 0.6840 0.092 Uiso 1 1 calc R U . . .
C3 C 0.6459(6) 0.0377(6) 0.7915(4) 0.0479(16) Uani 1 1 d . U . . .
C56 C 0.2482(7) 0.2491(7) 0.1126(5) 0.064(2) Uani 1 1 d . U . . .
H56A H 0.2073 0.2751 0.0713 0.095 Uiso 1 1 calc R U . . .
H56B H 0.3064 0.2422 0.0971 0.095 Uiso 1 1 calc R U . . .
H56C H 0.1928 0.1800 0.1111 0.095 Uiso 1 1 calc R U . . .
C30 C 0.2754(6) 0.1977(7) 0.4747(5) 0.069(2) Uani 1 1 d . U . . .
H30A H 0.1969 0.1872 0.4585 0.104 Uiso 1 1 calc R U . . .
H30B H 0.2968 0.2094 0.4271 0.104 Uiso 1 1 calc R U . . .
H30C H 0.2779 0.1349 0.4867 0.104 Uiso 1 1 calc R U . . .
C5 C 0.7399(6) 0.2172(6) 0.7789(4) 0.0499(17) Uani 1 1 d . U . . .
C6 C 0.8301(6) 0.1983(6) 0.7760(4) 0.0512(17) Uani 1 1 d . U . . .
H6 H 0.8938 0.2533 0.7730 0.061 Uiso 1 1 calc R U . . .
C12 C 0.5759(7) 0.2111(6) 0.8705(4) 0.0573(19) Uani 1 1 d . U . . .
C2 C 0.7384(6) 0.0230(6) 0.7886(4) 0.0507(17) Uani 1 1 d . U . . .
H2 H 0.7388 -0.0406 0.7943 0.061 Uiso 1 1 calc R U . . .
C29 C 0.3538(7) 0.3959(7) 0.5392(6) 0.064(2) Uani 1 1 d . U . . .
H29A H 0.2745 0.3829 0.5229 0.096 Uiso 1 1 calc R U . . .
H29B H 0.4067 0.4569 0.5917 0.096 Uiso 1 1 calc R U . . .
H29C H 0.3755 0.4102 0.4921 0.096 Uiso 1 1 calc R U . . .
C15 C 0.5540(10) 0.3904(9) 0.9644(7) 0.093(3) Uani 1 1 d . U . . .
H15A H 0.5457 0.4276 1.0110 0.139 Uiso 1 1 calc R U . . .
H15B H 0.6335 0.4024 0.9852 0.139 Uiso 1 1 calc R U . . .
H15C H 0.5367 0.4171 0.9152 0.139 Uiso 1 1 calc R U . . .
C55 C 0.3949(8) 0.4388(7) 0.2062(7) 0.085(3) Uani 1 1 d . U . . .
H55A H 0.3531 0.4635 0.1641 0.127 Uiso 1 1 calc R U . . .
H55B H 0.4317 0.4891 0.2642 0.127 Uiso 1 1 calc R U . . .
H55C H 0.4544 0.4334 0.1915 0.127 Uiso 1 1 calc R U . . .
C16 C 0.4897(11) 0.2273(9) 1.0126(7) 0.098(3) Uani 1 1 d . U . . .
H16A H 0.4794 0.2653 1.0575 0.146 Uiso 1 1 calc R U . . .
H16B H 0.4347 0.1516 0.9939 0.146 Uiso 1 1 calc R U . . .
H16C H 0.5688 0.2383 1.0359 0.146 Uiso 1 1 calc R U . . .
C54 C 0.2194(9) 0.3357(10) 0.2332(6) 0.087(3) Uani 1 1 d . U . . .
H54A H 0.1749 0.3607 0.1937 0.130 Uiso 1 1 calc R U . . .
H54B H 0.1669 0.2660 0.2329 0.130 Uiso 1 1 calc R U . . .
H54C H 0.2600 0.3856 0.2918 0.130 Uiso 1 1 calc R U . . .
C8 C 0.9136(9) -0.0249(8) 0.7704(7) 0.082(3) Uani 1 1 d . U . . .
H8A H 0.8495 -0.0718 0.7140 0.123 Uiso 1 1 calc R U . . .
H8B H 0.9830 -0.0291 0.7752 0.123 Uiso 1 1 calc R U . . .
H8C H 0.8931 -0.0466 0.8163 0.123 Uiso 1 1 calc R U . . .
C01H C 1.1414(11) 0.8434(10) 0.9790(8) 0.098(3) Uani 1 1 d D U . . .
C10 C 0.9648(12) 0.1170(11) 0.7038(10) 0.110(4) Uani 1 1 d . U . . .
H10A H 0.8957 0.0721 0.6493 0.165 Uiso 1 1 calc R U . . .
H10B H 0.9881 0.1915 0.7092 0.165 Uiso 1 1 calc R U . . .
H10C H 1.0279 0.1037 0.7043 0.165 Uiso 1 1 calc R U . . .
C9 C 1.0376(10) 0.1555(14) 0.8687(9) 0.159(8) Uani 1 1 d . U . . .
H9A H 1.0125 0.1339 0.9128 0.238 Uiso 1 1 calc R U . . .
H9B H 1.1023 0.1430 0.8729 0.238 Uiso 1 1 calc R U . . .
H9C H 1.0625 0.2308 0.8778 0.238 Uiso 1 1 calc R U . . .
C14 C 0.3452(10) 0.2495(14) 0.8941(9) 0.135(6) Uani 1 1 d . U . . .
H14A H 0.3294 0.2836 0.9373 0.203 Uiso 1 1 calc R U . . .
H14B H 0.3351 0.2790 0.8461 0.203 Uiso 1 1 calc R U . . .
H14C H 0.2914 0.1733 0.8722 0.203 Uiso 1 1 calc R U . . .
C36 C 1.1492(10) 0.5812(14) 0.6841(13) 0.160(8) Uani 1 1 d . U . . .
H36A H 1.2312 0.6345 0.7099 0.240 Uiso 1 1 calc R U . . .
H36B H 1.1226 0.5499 0.6221 0.240 Uiso 1 1 calc R U . . .
H36C H 1.1041 0.6147 0.6925 0.240 Uiso 1 1 calc R U . . .
C35 C 1.1982(10) 0.4377(11) 0.7117(13) 0.147(7) Uani 1 1 d . U . . .
H35A H 1.2811 0.4880 0.7363 0.221 Uiso 1 1 calc R U . . .
H35B H 1.1857 0.3824 0.7396 0.221 Uiso 1 1 calc R U . . .
H35C H 1.1693 0.4055 0.6495 0.221 Uiso 1 1 calc R U . . .
C34 C 1.1759(10) 0.5351(15) 0.8242(8) 0.149(7) Uani 1 1 d . U . . .
H34A H 1.2579 0.5887 0.8509 0.224 Uiso 1 1 calc R U . . .
H34B H 1.1312 0.5663 0.8375 0.224 Uiso 1 1 calc R U . . .
H34C H 1.1662 0.4757 0.8471 0.224 Uiso 1 1 calc R U . . .
C48 C 0.9626(13) 0.2204(18) 0.3666(15) 0.194(10) Uani 1 1 d . U . . .
H48A H 0.9229 0.2107 0.3051 0.292 Uiso 1 1 calc R U . . .
H48B H 0.9918 0.2932 0.4006 0.292 Uiso 1 1 calc R U . . .
H48C H 1.0274 0.2063 0.3764 0.292 Uiso 1 1 calc R U . . .
Cl01 Cl 0.8900(2) 0.5724(2) 0.98681(16) 0.0856(8) Uani 1 1 d D U . . .
Cl02 Cl 1.1213(4) 0.9563(3) 0.9728(3) 0.1314(13) Uani 1 1 d . U . . .
Cl00 Cl 1.3051(5) 0.9000(5) 0.9137(4) 0.184(2) Uani 1 1 d D U . . .
C01P C 1.1719(14) 0.8053(11) 0.9134(10) 0.133(5) Uani 1 1 d D U . . .
C01Q C 1.0113(10) 0.5505(7) 0.9881(8) 0.188(10) Uani 1 1 d D U . . .
C50 C 0.9382(16) 0.159(2) 0.4879(8) 0.209(11) Uani 1 1 d . U . . .
H50A H 0.9664 0.2313 0.5217 0.314 Uiso 1 1 calc R U . . .
H50B H 0.8849 0.1090 0.5061 0.314 Uiso 1 1 calc R U . . .
H50C H 1.0039 0.1460 0.4976 0.314 Uiso 1 1 calc R U . . .
C49 C 0.8365(13) 0.0310(12) 0.3470(19) 0.250(15) Uani 1 1 d . U . . .
H49A H 0.7954 0.0173 0.2848 0.375 Uiso 1 1 calc R U . . .
H49B H 0.9033 0.0198 0.3582 0.375 Uiso 1 1 calc R U . . .
H49C H 0.7843 -0.0172 0.3667 0.375 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6350(8) 0.0285(7) 0.4917(7) 0.112(2) Uani 0.5 1 d D U P A 1
C0AA C 0.5462(16) -0.0357(14) 0.5408(12) 0.087(6) Uani 0.5 1 d D U P A 1
C1AA C 0.5340(17) -0.0127(18) 0.4543(10) 0.088(6) Uani 0.5 1 d D U P B 2
Cl2 Cl 0.6515(7) 0.0342(8) 0.5571(5) 0.125(3) Uani 0.5 1 d D U P B 2
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'
Cl Cl 0.3639 0.7018 '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'
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
C32 O21 C24 118.9(5) . .
C52 O41 C41 117.6(4) . .
C4 O1 C12 116.4(5) . .
C12 N1 C13 126.2(6) . .
C12 N1 H1 116.9 . .
C13 N1 H1 116.9 . .
C32 N21 C33 126.2(6) . .
C32 N21 H21 116.9 . .
C33 N21 H21 116.9 . .
C52 N41 C53 124.3(5) . .
C52 N41 H41 117.8 . .
C53 N41 H41 117.8 . .
C46 C41 O41 120.1(5) . .
C46 C41 C42 121.9(5) . .
O41 C41 C42 118.0(5) . .
C43 C42 C41 118.0(5) . .
C43 C42 C31 121.6(5) . .
C41 C42 C31 120.3(5) . .
C23 C24 O21 119.6(5) . .
C23 C24 C25 121.4(5) . .
O21 C24 C25 118.9(5) . .
C22 C23 C24 118.3(5) . .
C22 C23 C11 121.1(5) . .
C24 C23 C11 120.7(5) . .
C26 C25 C24 117.8(5) . .
C26 C25 C31 121.8(5) . .
C24 C25 C31 120.4(5) . .
C25 C31 C42 115.5(5) . .
C25 C31 H31A 108.4 . .
C42 C31 H31A 108.4 . .
C25 C31 H31B 108.4 . .
C42 C31 H31B 108.4 . .
H31A C31 H31B 107.5 . .
C45 C46 C41 117.5(5) . .
C45 C46 C51 121.0(6) . .
C41 C46 C51 121.5(6) . .
O42 C52 N41 128.8(6) . .
O42 C52 O41 123.0(5) . .
N41 C52 O41 108.2(5) . .
C42 C43 C44 123.2(6) . .
C42 C43 H43 118.4 . .
C44 C43 H43 118.4 . .
C26 C21 C22 116.0(6) . .
C26 C21 C27 120.0(6) . .
C22 C21 C27 124.0(5) . .
O22 C32 N21 127.9(6) . .
O22 C32 O21 123.4(6) . .
N21 C32 O21 108.7(5) . .
C25 C26 C21 123.4(5) . .
C25 C26 H26 118.3 . .
C21 C26 H26 118.3 . .
C5 C11 C23 116.2(5) . .
C5 C11 H11A 108.2 . .
C23 C11 H11A 108.2 . .
C5 C11 H11B 108.2 . .
C23 C11 H11B 108.2 . .
H11A C11 H11B 107.4 . .
C46 C45 C44 123.0(6) . .
C46 C45 H45 118.5 . .
C44 C45 H45 118.5 . .
C43 C44 C45 116.4(6) . .
C43 C44 C47 122.3(6) . .
C45 C44 C47 121.3(6) . .
C46 C51 C3 115.3(5) . 2_656
C46 C51 H51A 108.4 . .
C3 C51 H51A 108.4 2_656 .
C46 C51 H51B 108.4 . .
C3 C51 H51B 108.4 2_656 .
H51A C51 H51B 107.5 . .
C23 C22 C21 122.9(5) . .
C23 C22 H22 118.5 . .
C21 C22 H22 118.5 . .
C2 C1 C6 116.8(7) . .
C2 C1 C7 124.5(7) . .
C6 C1 C7 118.1(6) . .
O1 C4 C3 121.7(6) . .
O1 C4 C5 120.5(6) . .
C3 C4 C5 117.8(6) . .
C21 C27 C30 109.8(5) . .
C21 C27 C29 111.2(6) . .
C30 C27 C29 109.8(6) . .
C21 C27 C28 111.4(6) . .
C30 C27 C28 108.3(6) . .
C29 C27 C28 106.4(6) . .
C9 C7 C10 115.3(10) . .
C9 C7 C1 109.3(6) . .
C10 C7 C1 112.2(7) . .
C9 C7 C8 104.4(9) . .
C10 C7 C8 105.7(7) . .
C1 C7 C8 109.5(6) . .
N41 C53 C56 110.2(6) . .
N41 C53 C54 105.3(6) . .
C56 C53 C54 111.4(7) . .
N41 C53 C55 109.9(6) . .
C56 C53 C55 109.7(7) . .
C54 C53 C55 110.3(8) . .
C50 C47 C49 106.7(15) . .
C50 C47 C48 109.0(14) . .
C49 C47 C48 110.2(15) . .
C50 C47 C44 111.4(6) . .
C49 C47 C44 110.9(7) . .
C48 C47 C44 108.6(7) . .
N21 C33 C36 109.7(7) . .
N21 C33 C34 108.5(7) . .
C36 C33 C34 114.8(12) . .
N21 C33 C35 106.4(7) . .
C36 C33 C35 111.3(11) . .
C34 C33 C35 105.9(11) . .
N1 C13 C14 104.9(8) . .
N1 C13 C16 112.2(7) . .
C14 C13 C16 111.7(9) . .
N1 C13 C15 108.4(7) . .
C14 C13 C15 109.4(10) . .
C16 C13 C15 110.1(8) . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C2 C3 C4 121.2(6) . .
C2 C3 C51 122.2(6) . 2_656
C4 C3 C51 116.5(6) . 2_656
C53 C56 H56A 109.5 . .
C53 C56 H56B 109.5 . .
H56A C56 H56B 109.5 . .
C53 C56 H56C 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
C27 C30 H30A 109.5 . .
C27 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C27 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C6 C5 C4 118.7(6) . .
C6 C5 C11 122.7(6) . .
C4 C5 C11 118.6(6) . .
C5 C6 C1 123.2(7) . .
C5 C6 H6 118.4 . .
C1 C6 H6 118.4 . .
O2 C12 N1 128.6(7) . .
O2 C12 O1 121.6(7) . .
N1 C12 O1 109.8(6) . .
C1 C2 C3 122.1(7) . .
C1 C2 H2 119.0 . .
C3 C2 H2 119.0 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C53 C55 H55A 109.5 . .
C53 C55 H55B 109.5 . .
H55A C55 H55B 109.5 . .
C53 C55 H55C 109.5 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C01P C01H Cl02 115.4(9) . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C33 C36 H36A 109.5 . .
C33 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C33 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C33 C35 H35A 109.5 . .
C33 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C33 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C47 C48 H48A 109.5 . .
C47 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
C47 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C01H C01P Cl00 115.3(11) . .
C01Q C01Q Cl01 104.9(10) 2_767 .
C47 C50 H50A 109.5 . .
C47 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
C47 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C47 C49 H49A 109.5 . .
C47 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
C47 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O21 C32 1.371(8) .
O21 C24 1.395(7) .
O41 C52 1.381(7) .
O41 C41 1.398(7) .
O42 C52 1.204(7) .
O1 C4 1.331(8) .
O1 C12 1.404(9) .
O2 C12 1.206(9) .
O22 C32 1.180(8) .
N1 C12 1.280(10) .
N1 C13 1.459(9) .
N1 H1 0.8600 .
N21 C32 1.319(8) .
N21 C33 1.464(9) .
N21 H21 0.8600 .
N41 C52 1.333(8) .
N41 C53 1.490(8) .
N41 H41 0.8600 .
C41 C46 1.382(8) .
C41 C42 1.400(8) .
C42 C43 1.368(9) .
C42 C31 1.541(8) .
C24 C23 1.383(8) .
C24 C25 1.404(8) .
C23 C22 1.381(9) .
C23 C11 1.529(8) .
C25 C26 1.372(9) .
C25 C31 1.510(8) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C46 C45 1.380(9) .
C46 C51 1.515(9) .
C43 C44 1.380(9) .
C43 H43 0.9300 .
C21 C26 1.398(9) .
C21 C22 1.400(9) .
C21 C27 1.509(9) .
C26 H26 0.9300 .
C11 C5 1.503(9) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C45 C44 1.405(9) .
C45 H45 0.9300 .
C44 C47 1.536(9) .
C51 C3 1.558(9) 2_656
C51 H51A 0.9700 .
C51 H51B 0.9700 .
C22 H22 0.9300 .
C1 C2 1.382(10) .
C1 C6 1.412(11) .
C1 C7 1.530(10) .
C4 C3 1.407(9) .
C4 C5 1.436(10) .
C27 C30 1.520(10) .
C27 C29 1.543(10) .
C27 C28 1.559(10) .
C7 C9 1.484(13) .
C7 C10 1.506(13) .
C7 C8 1.534(12) .
C53 C56 1.501(10) .
C53 C54 1.503(12) .
C53 C55 1.538(11) .
C47 C50 1.454(15) .
C47 C49 1.470(16) .
C47 C48 1.511(14) .
C33 C36 1.477(14) .
C33 C34 1.489(14) .
C33 C35 1.511(14) .
C13 C14 1.480(14) .
C13 C16 1.504(14) .
C13 C15 1.535(14) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C3 C2 1.391(10) .
C3 C51 1.558(9) 2_656
C56 H56A 0.9600 .
C56 H56B 0.9600 .
C56 H56C 0.9600 .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C5 C6 1.391(10) .
C6 H6 0.9300 .
C2 H2 0.9300 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C55 H55A 0.9600 .
C55 H55B 0.9600 .
C55 H55C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C54 H54A 0.9600 .
C54 H54B 0.9600 .
C54 H54C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C01H C01P 1.435(14) .
C01H Cl02 1.758(11) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C36 H36A 0.9600 .
C36 H36B 0.9600 .
C36 H36C 0.9600 .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C34 H34A 0.9600 .
C34 H34B 0.9600 .
C34 H34C 0.9600 .
C48 H48A 0.9600 .
C48 H48B 0.9600 .
C48 H48C 0.9600 .
Cl01 C01Q 1.816(12) .
Cl00 C01P 1.775(14) .
C01Q C01Q 1.488(16) 2_767
C50 H50A 0.9600 .
C50 H50B 0.9600 .
C50 H50C 0.9600 .
C49 H49A 0.9600 .
C49 H49B 0.9600 .
C49 H49C 0.9600 .
Cl1 C0AA 1.732(13) .
C1AA C0AA 1.544(7) 2_656
C1AA Cl2 1.735(14) .
