#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/20/7012022.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_7012022
loop_
_publ_author_name
'Volkmer, Dirk'
'Fricke, Marc'
'Vollhardt, Dieter'
'Siegel, Stefan'
_publ_section_title
;
 Crystallization of (012) oriented calcite single crystals underneath
 monolayers of tetra(carboxymethoxy)calix[4]arenes
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4547
_journal_paper_doi               10.1039/b206912a
_journal_year                    2002
_chemical_formula_sum            'C72.75 H115.5 O17'
_chemical_formula_weight         1262.15
_chemical_name_systematic
; 
5,11,17,23-tetrakis-(1,1,3,3-tetramethylbutyl)-25,26,27,28-
tetra(carboxymethoxy)calix[4]arene 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.2510(10)
_cell_angle_beta                 93.3370(10)
_cell_angle_gamma                107.2020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2924(5)
_cell_length_b                   12.8365(5)
_cell_length_c                   25.2557(11)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.16
_cell_volume                     3757.2(3)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics
'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker AXS SMART'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            38412
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.9696
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .08
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         16065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0956P)²+1.7806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                9892
_reflns_number_total             16065
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b206912a.txt
_cod_data_source_block           frick
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C72.75 H115.50 O17'
_cod_database_code               7012022
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.87676(13) 0.36073(13) 0.15804(6) 0.0294(4) Uani 1 1 d . . .
O2 O 0.72866(19) 0.41695(18) 0.09681(8) 0.0529(6) Uani 1 1 d . . .
H2 H 0.7531 0.4324 0.1295 0.079 Uiso 1 1 calc R . .
O3 O 0.7286(2) 0.2948(2) 0.02875(9) 0.0679(7) Uani 1 1 d . . .
O4 O 0.96204(13) 0.59140(14) 0.12769(6) 0.0307(4) Uani 1 1 d . . .
O5 O 0.99236(19) 0.6689(2) -0.00252(8) 0.0574(6) Uani 1 1 d . . .
H5 H 0.9789 0.7195 -0.0173 0.086 Uiso 1 1 calc R . .
O6 O 0.9382(2) 0.7531(2) 0.06885(9) 0.0672(7) Uani 1 1 d . . .
O7 O 0.74394(14) 0.58952(13) 0.18013(6) 0.0302(4) Uani 1 1 d . . .
O8 O 0.5620(2) 0.6484(2) 0.08001(10) 0.0762(8) Uani 1 1 d . . .
H8 H 0.4932 0.6205 0.0673 0.114 Uiso 1 1 calc R . .
O9 O 0.51215(18) 0.53186(18) 0.13965(9) 0.0586(6) Uani 1 1 d . . .
O10 O 0.65298(13) 0.33591(13) 0.19238(6) 0.0297(4) Uani 1 1 d . . .
O11 O 0.39495(15) 0.15367(18) 0.12087(9) 0.0564(6) Uani 1 1 d . . .
H11 H 0.3794 0.0938 0.0999 0.085 Uiso 1 1 calc R . .
O12 O 0.57395(16) 0.14639(17) 0.11950(9) 0.0533(6) Uani 1 1 d . . .
C1 C 0.91054(18) 0.24767(18) 0.22218(9) 0.0260(5) Uani 1 1 d . . .
C2 C 0.9889(2) 0.2122(2) 0.25162(10) 0.0302(5) Uani 1 1 d . . .
H2A H 0.9608 0.1578 0.2739 0.036 Uiso 1 1 calc . . .
C3 C 1.10645(19) 0.2534(2) 0.24972(10) 0.0297(5) Uani 1 1 d . . .
C4 C 1.14485(19) 0.3344(2) 0.21711(10) 0.0307(5) Uani 1 1 d . . .
H4 H 1.2249 0.3649 0.2157 0.037 Uiso 1 1 calc . . .
C5 C 1.07059(19) 0.37218(19) 0.18670(9) 0.0266(5) Uani 1 1 d . . .
C6 C 0.95305(19) 0.32603(19) 0.18938(9) 0.0259(5) Uani 1 1 d . . .
C7 C 1.1924(2) 0.2107(2) 0.28015(11) 0.0356(6) Uani 1 1 d . . .
C8 C 1.2548(3) 0.1599(3) 0.23774(13) 0.0529(8) Uani 1 1 d . . .
H8A H 1.1988 0.0997 0.2136 0.079 Uiso 1 1 calc R . .
H8B H 1.3102 0.1312 0.2556 0.079 Uiso 1 1 calc R . .
H8C H 1.2949 0.2166 0.2170 0.079 Uiso 1 1 calc R . .
C9 C 1.1330(3) 0.1173(3) 0.31117(14) 0.0532(8) Uani 1 1 d . . .
H9A H 1.0848 0.1432 0.3360 0.080 Uiso 1 1 calc R . .
H9B H 1.1910 0.0956 0.3315 0.080 Uiso 1 1 calc R . .
H9C H 1.0854 0.0538 0.2858 0.080 Uiso 1 1 calc R . .
C10 C 1.2855(2) 0.3047(2) 0.31711(11) 0.0408(6) Uani 1 1 d . . .
H10A H 1.3445 0.2720 0.3291 0.049 Uiso 1 1 calc . . .
H10B H 1.3222 0.3589 0.2939 0.049 Uiso 1 1 calc . . .
C11 C 1.2610(3) 0.3718(3) 0.36761(12) 0.0498(7) Uani 1 1 d . . .
C12 C 1.1679(3) 0.4252(3) 0.35584(15) 0.0645(10) Uani 1 1 d . . .
H12A H 1.1866 0.4666 0.3258 0.097 Uiso 1 1 calc R . .
H12B H 1.1636 0.4754 0.3877 0.097 Uiso 1 1 calc R . .
H12C H 1.0940 0.3677 0.3465 0.097 Uiso 1 1 calc R . .
C13 C 1.3732(3) 0.4628(3) 0.38768(14) 0.0622(9) Uani 1 1 d . . .
H13A H 1.4333 0.4295 0.3957 0.093 Uiso 1 1 calc R . .
H13B H 1.3628 0.5075 0.4203 0.093 Uiso 1 1 calc R . .
H13C H 1.3955 0.5098 0.3599 0.093 Uiso 1 1 calc R . .
C14 C 1.2318(5) 0.3044(4) 0.41406(16) 0.0947(15) Uani 1 1 d . . .
H14A H 1.1519 0.2574 0.4076 0.142 Uiso 1 1 calc R . .
H14B H 1.2427 0.3547 0.4479 0.142 Uiso 1 1 calc R . .
H14C H 1.2822 0.2582 0.4162 0.142 Uiso 1 1 calc R . .
C15 C 0.8385(2) 0.2913(2) 0.10775(10) 0.0356(6) Uani 1 1 d . . .
H15A H 0.7966 0.2157 0.1137 0.043 Uiso 1 1 calc . . .
H15B H 0.9053 0.2878 0.0883 0.043 Uiso 1 1 calc . . .
C16 C 0.7613(2) 0.3351(2) 0.07466(10) 0.0381(6) Uani 1 1 d . . .
C17 C 1.1159(2) 0.4624(2) 0.15283(10) 0.0307(5) Uani 1 1 d . . .
H17A H 1.0646 0.4470 0.1192 0.037 Uiso 1 1 calc . . .
H17B H 1.1927 0.4618 0.1431 0.037 Uiso 1 1 calc . . .
C18 C 1.12437(19) 0.5761(2) 0.18207(10) 0.0294(5) Uani 1 1 d . . .
C19 C 1.2127(2) 0.6264(2) 0.22263(10) 0.0353(6) Uani 1 1 d . . .
H19 H 1.2680 0.5902 0.2295 0.042 Uiso 1 1 calc . . .
C20 C 1.2238(2) 0.7277(2) 0.25365(10) 0.0374(6) Uani 1 1 d . . .
C21 C 1.1358(2) 0.7730(2) 0.24543(10) 0.0353(6) Uani 1 1 d . . .
H21 H 1.1371 0.8382 0.2683 0.042 Uiso 1 1 calc . . .
C22 C 1.0455(2) 0.7270(2) 0.20516(10) 0.0305(5) Uani 1 1 d . . .
C23 C 1.04478(19) 0.63172(19) 0.17137(9) 0.0279(5) Uani 1 1 d . . .
C24 C 1.3292(2) 0.7852(2) 0.29429(11) 0.0431(7) Uani 1 1 d . . .
C25 C 1.3207(3) 0.8980(3) 0.32434(15) 0.0734(11) Uani 1 1 d . . .
H25A H 1.2570 0.8831 0.3468 0.110 Uiso 1 1 calc R . .
H25B H 1.3074 0.9437 0.2979 0.110 Uiso 1 1 calc R . .
H25C H 1.3923 0.9370 0.3470 0.110 Uiso 1 1 calc R . .
C26 C 1.3276(4) 0.7171(4) 0.33795(17) 0.1060(18) Uani 1 1 d . . .
H26A H 1.2521 0.6989 0.3514 0.159 Uiso 1 1 calc R . .
H26B H 1.3862 0.7587 0.3672 0.159 Uiso 1 1 calc R . .
H26C H 1.3436 0.6490 0.3239 0.159 Uiso 1 1 calc R . .
C27 C 1.4410(3) 0.8044(3) 0.26878(14) 0.0559(8) Uani 1 1 d . . .
H27A H 1.4435 0.7308 0.2529 0.067 Uiso 1 1 calc . . .
H27B H 1.5028 0.8316 0.2987 0.067 Uiso 1 1 calc . . .
C28 C 1.4771(2) 0.8811(3) 0.22544(12) 0.0483(7) Uani 1 1 d . . .
C29 C 1.5143(4) 1.0047(3) 0.2477(2) 0.0970(16) Uani 1 1 d . . .
H29A H 1.5383 1.0476 0.2186 0.145 Uiso 1 1 calc R . .
H29B H 1.5783 1.0216 0.2756 0.145 Uiso 1 1 calc R . .
H29C H 1.4499 1.0236 0.2630 0.145 Uiso 1 1 calc R . .
C30 C 1.5882(3) 0.8608(4) 0.20900(19) 0.0845(12) Uani 1 1 d . . .
H30A H 1.5722 0.7831 0.1937 0.127 Uiso 1 1 calc R . .
H30B H 1.6442 0.8787 0.2406 0.127 Uiso 1 1 calc R . .
H30C H 1.6190 0.9076 0.1822 0.127 Uiso 1 1 calc R . .
C31 C 1.3897(3) 0.8522(5) 0.17754(17) 0.117(2) Uani 1 1 d . . .
H31A H 1.3163 0.8570 0.1891 0.176 Uiso 1 1 calc R . .
H31B H 1.3802 0.7769 0.1602 0.176 Uiso 1 1 calc R . .
H31C H 1.4154 0.9038 0.1520 0.176 Uiso 1 1 calc R . .
C32 C 1.0036(2) 0.5948(2) 0.07635(10) 0.0394(6) Uani 1 1 d . . .
H32A H 0.9703 0.5217 0.0540 0.047 Uiso 1 1 calc . . .
H32B H 1.0878 0.6109 0.0806 0.047 Uiso 1 1 calc . . .
C33 C 0.9738(2) 0.6819(3) 0.04783(12) 0.0470(7) Uani 1 1 d . . .
C34 C 0.9517(2) 0.7805(2) 0.19902(10) 0.0317(5) Uani 1 1 d . . .
H34A H 0.9124 0.7565 0.1622 0.038 Uiso 1 1 calc . . .
H34B H 0.9867 0.8616 0.2038 0.038 Uiso 1 1 calc . . .
C35 C 0.8640(2) 0.75187(19) 0.23913(9) 0.0281(5) Uani 1 1 d . . .
C36 C 0.8793(2) 0.81930(19) 0.28819(10) 0.0315(5) Uani 1 1 d . . .
H36 H 0.9420 0.8853 0.2946 0.038 Uiso 1 1 calc . . .
C37 C 0.8068(2) 0.7949(2) 0.32863(10) 0.0313(5) Uani 1 1 d . . .
C38 C 0.7183(2) 0.6962(2) 0.31857(10) 0.0296(5) Uani 1 1 d . . .
H38 H 0.6691 0.6765 0.3457 0.036 Uiso 1 1 calc . . .
C39 C 0.69851(19) 0.62472(19) 0.27006(9) 0.0267(5) Uani 1 1 d . . .
C40 C 0.76863(19) 0.65644(19) 0.23001(9) 0.0268(5) Uani 1 1 d . . .
C41 C 0.8260(2) 0.8769(2) 0.38070(11) 0.0378(6) Uani 1 1 d . . .
C42 C 0.8121(3) 0.9854(2) 0.36558(13) 0.0497(7) Uani 1 1 d . . .
H42A H 0.8704 1.0156 0.3421 0.075 Uiso 1 1 calc R . .
H42B H 0.8214 1.0386 0.3982 0.075 Uiso 1 1 calc R . .
H42C H 0.7358 0.9707 0.3469 0.075 Uiso 1 1 calc R . .
C43 C 0.7349(3) 0.8365(3) 0.41904(12) 0.0526(8) Uani 1 1 d . . .
H43A H 0.6592 0.8311 0.4021 0.079 Uiso 1 1 calc R . .
H43B H 0.7521 0.8888 0.4525 0.079 Uiso 1 1 calc R . .
H43C H 0.7353 0.7638 0.4270 0.079 Uiso 1 1 calc R . .
C44 C 0.9500(2) 0.9072(2) 0.40838(10) 0.0374(6) Uani 1 1 d . . .
H44A H 1.0013 0.9401 0.3821 0.045 Uiso 1 1 calc . . .
H44B H 0.9571 0.9674 0.4383 0.045 Uiso 1 1 calc . . .
C45 C 1.0025(3) 0.8252(2) 0.43146(11) 0.0458(7) Uani 1 1 d . . .
C46 C 1.1282(3) 0.8904(3) 0.45020(14) 0.0623(9) Uani 1 1 d . . .
H46A H 1.1315 0.9524 0.4779 0.093 Uiso 1 1 calc R . .
H46B H 1.1666 0.9186 0.4197 0.093 Uiso 1 1 calc R . .
H46C H 1.1665 0.8420 0.4650 0.093 Uiso 1 1 calc R . .
C47 C 0.9997(3) 0.7260(3) 0.39004(13) 0.0538(8) Uani 1 1 d . . .
H47A H 1.0353 0.7522 0.3585 0.081 Uiso 1 1 calc R . .
H47B H 0.9201 0.6809 0.3793 0.081 Uiso 1 1 calc R . .
H47C H 1.0418 0.6816 0.4058 0.081 Uiso 1 1 calc R . .
C48 C 0.9472(3) 0.7838(3) 0.48076(14) 0.0686(10) Uani 1 1 d . . .
H48A H 0.9930 0.7444 0.4980 0.103 Uiso 1 1 calc R . .
H48B H 0.8696 0.7339 0.4696 0.103 Uiso 1 1 calc R . .
H48C H 0.9435 0.8468 0.5061 0.103 Uiso 1 1 calc R . .
C49 C 0.7093(2) 0.6405(2) 0.13775(10) 0.0379(6) Uani 1 1 d . . .
H49A H 0.7513 0.6281 0.1065 0.046 Uiso 1 1 calc . . .
H49B H 0.7310 0.7210 0.1497 0.046 Uiso 1 1 calc . . .
C50 C 0.5829(3) 0.5979(3) 0.12044(12) 0.0474(7) Uani 1 1 d . . .
C51 C 0.60626(19) 0.51347(19) 0.26314(10) 0.0288(5) Uani 1 1 d . . .
H51A H 0.5764 0.4903 0.2248 0.035 Uiso 1 1 calc . . .
H51B H 0.5420 0.5196 0.2839 0.035 Uiso 1 1 calc . . .
C52 C 0.65578(18) 0.42782(19) 0.28257(9) 0.0267(5) Uani 1 1 d . . .
C53 C 0.6821(2) 0.43214(19) 0.33745(10) 0.0300(5) Uani 1 1 d . . .
H53 H 0.6622 0.4847 0.3618 0.036 Uiso 1 1 calc . . .
C54 C 0.7362(2) 0.3628(2) 0.35812(10) 0.0303(5) Uani 1 1 d . . .
C55 C 0.76814(19) 0.2902(2) 0.32113(10) 0.0296(5) Uani 1 1 d . . .
H55 H 0.8091 0.2449 0.3341 0.036 Uiso 1 1 calc . . .
C56 C 0.74296(18) 0.28096(18) 0.26605(9) 0.0262(5) Uani 1 1 d . . .
C57 C 0.68242(18) 0.34773(19) 0.24737(9) 0.0257(5) Uani 1 1 d . . .
C58 C 0.7650(2) 0.3677(2) 0.41877(10) 0.0378(6) Uani 1 1 d . . .
C59 C 0.8969(3) 0.4005(3) 0.42949(13) 0.0528(8) Uani 1 1 d . . .
H59A H 0.9188 0.4119 0.4682 0.079 Uiso 1 1 calc R . .
H59B H 0.9316 0.4688 0.4151 0.079 Uiso 1 1 calc R . .
H59C H 0.9238 0.3415 0.4119 0.079 Uiso 1 1 calc R . .
C60 C 0.7280(3) 0.4572(3) 0.45205(12) 0.0536(8) Uani 1 1 d . . .
H60A H 0.6460 0.4445 0.4433 0.080 Uiso 1 1 calc R . .
H60B H 0.7711 0.5297 0.4438 0.080 Uiso 1 1 calc R . .
H60C H 0.7433 0.4547 0.4903 0.080 Uiso 1 1 calc R . .
C61 C 0.7178(2) 0.2538(2) 0.43732(11) 0.0397(6) Uani 1 1 d . . .
H61A H 0.7560 0.2604 0.4737 0.048 Uiso 1 1 calc . . .
H61B H 0.7456 0.2016 0.4137 0.048 Uiso 1 1 calc . . .
C62 C 0.5886(2) 0.1960(2) 0.44008(11) 0.0431(7) Uani 1 1 d . . .
C63 C 0.5773(3) 0.0749(3) 0.44503(16) 0.0649(10) Uani 1 1 d . . .
H63A H 0.6253 0.0721 0.4769 0.097 Uiso 1 1 calc R . .
H63B H 0.6022 0.0405 0.4130 0.097 Uiso 1 1 calc R . .
H63C H 0.4972 0.0349 0.4484 0.097 Uiso 1 1 calc R . .
C64 C 0.5430(3) 0.2445(4) 0.48917(15) 0.0778(12) Uani 1 1 d . . .
H64A H 0.4650 0.1984 0.4921 0.117 Uiso 1 1 calc R . .
H64B H 0.5426 0.3194 0.4854 0.117 Uiso 1 1 calc R . .
H64C H 0.5924 0.2468 0.5215 0.117 Uiso 1 1 calc R . .
C65 C 0.5157(2) 0.1960(3) 0.38956(13) 0.0524(8) Uani 1 1 d . . .
H65A H 0.5461 0.1656 0.3582 0.079 Uiso 1 1 calc R . .
H65B H 0.5172 0.2718 0.3865 0.079 Uiso 1 1 calc R . .
H65C H 0.4367 0.1507 0.3913 0.079 Uiso 1 1 calc R . .
C66 C 0.5338(2) 0.2943(2) 0.17545(11) 0.0380(6) Uani 1 1 d . . .
H66A H 0.5095 0.3507 0.1589 0.046 Uiso 1 1 calc . . .
H66B H 0.4910 0.2794 0.2071 0.046 Uiso 1 1 calc . . .
C67 C 0.5050(2) 0.1899(2) 0.13568(11) 0.0375(6) Uani 1 1 d . . .
C68 C 0.78319(19) 0.20234(19) 0.22797(10) 0.0282(5) Uani 1 1 d . . .
H68A H 0.7394 0.1892 0.1923 0.034 Uiso 1 1 calc . . .
H68B H 0.7678 0.1308 0.2415 0.034 Uiso 1 1 calc . . .
O13 O 0.3292(2) -0.0296(2) 0.05744(9) 0.0656(6) Uani 1 1 d . . .
H13 H 0.3407 -0.0300 0.0250 0.098 Uiso 1 1 calc R . .
C69 C 0.2186(3) -0.1015(3) 0.06160(17) 0.0718(10) Uani 1 1 d . . .
H69A H 0.1983 -0.0888 0.0983 0.108 Uiso 1 1 calc R . .
H69B H 0.2183 -0.1782 0.0528 0.108 Uiso 1 1 calc R . .
H69C H 0.1626 -0.0872 0.0365 0.108 Uiso 1 1 calc R . .
O14 O 0.6265(3) -0.0003(2) 0.04282(11) 0.0839(8) Uani 1 1 d . . .
H14 H 0.6019 0.0362 0.0666 0.126 Uiso 1 1 calc R . .
C70 C 0.5709(5) -0.1148(3) 0.04171(19) 0.0947(15) Uani 1 1 d . . .
H71A H 0.6045 -0.1575 0.0163 0.142 Uiso 1 1 calc R . .
H71B H 0.4891 -0.1315 0.0305 0.142 Uiso 1 1 calc R . .
H71C H 0.5807 -0.1342 0.0776 0.142 Uiso 1 1 calc R . .
O15 O 0.3474(3) 0.5975(3) 0.04589(13) 0.0982(10) Uani 1 1 d . . .
H15 H 0.3411 0.6303 0.0197 0.147 Uiso 1 1 calc R . .
C71 C 0.3027(4) 0.4839(4) 0.02978(19) 0.0963(15) Uani 1 1 d . . .
H70A H 0.3319 0.4454 0.0557 0.145 Uiso 1 1 calc R . .
H70B H 0.3259 0.4644 -0.0057 0.145 Uiso 1 1 calc R . .
H70C H 0.2190 0.4620 0.0279 0.145 Uiso 1 1 calc R . .
O16 O 0.9533(3) 0.8260(3) -0.05040(14) 0.1075(11) Uani 1 1 d . . .
H16 H 0.9674 0.8540 -0.0179 0.161 Uiso 1 1 calc R . .
C72 C 0.8418(4) 0.8169(4) -0.0678(2) 0.1135(18) Uani 1 1 d . . .
H72A H 0.8060 0.8464 -0.0382 0.170 Uiso 1 1 calc R . .
H72B H 0.7989 0.7391 -0.0798 0.170 Uiso 1 1 calc R . .
H72C H 0.8414 0.8587 -0.0976 0.170 Uiso 1 1 calc R . .
O17 O 1.0791(5) 1.0236(4) -0.0673(2) 0.1217(17) Uani 0.75 1 d P A 1
H17 H 1.0628 0.9619 -0.0567 0.183 Uiso 0.75 1 calc PR A 1
C73 C 1.1218(6) 1.0152(5) -0.1192(2) 0.0819(16) Uani 0.75 1 d P A 1
H73A H 1.1756 1.0864 -0.1234 0.123 Uiso 0.75 1 calc PR A 1
H73B H 1.0577 0.9946 -0.1473 0.123 Uiso 0.75 1 calc PR A 1
H73C H 1.1611 0.9588 -0.1220 0.123 Uiso 0.75 1 calc PR A 1
O18 O 1.1375(9) 0.9605(8) -0.0814(6) 0.081(3) Uani 0.25 1 d 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 0.0033 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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
C6 O1 C15 112.31(17) . . ?
C23 O4 C32 115.67(18) . . ?
C40 O7 C49 113.79(18) . . ?
C57 O10 C66 115.51(18) . . ?
C6 C1 C2 117.9(2) . . ?
C6 C1 C68 122.3(2) . . ?
C2 C1 C68 119.8(2) . . ?
C3 C2 C1 122.7(2) . . ?
C2 C3 C4 117.1(2) . . ?
C2 C3 C7 122.7(2) . . ?
C4 C3 C7 120.2(2) . . ?
C5 C4 C3 122.6(2) . . ?
C4 C5 C6 117.7(2) . . ?
C4 C5 C17 121.0(2) . . ?
C6 C5 C17 121.3(2) . . ?
C1 C6 O1 119.35(19) . . ?
C1 C6 C5 122.0(2) . . ?
O1 C6 C5 118.6(2) . . ?
C3 C7 C9 112.3(2) . . ?
C3 C7 C8 107.0(2) . . ?
C9 C7 C8 106.3(2) . . ?
C3 C7 C10 112.5(2) . . ?
C9 C7 C10 111.5(2) . . ?
C8 C7 C10 106.8(2) . . ?
C11 C10 C7 123.9(2) . . ?
C12 C11 C13 108.8(3) . . ?
C12 C11 C14 110.2(3) . . ?
C13 C11 C14 105.6(3) . . ?
C12 C11 C10 112.7(3) . . ?
C13 C11 C10 106.0(2) . . ?
C14 C11 C10 113.1(3) . . ?
O1 C15 C16 110.2(2) . . ?
O3 C16 O2 120.3(3) . . ?
O3 C16 C15 120.8(3) . . ?
O2 C16 C15 118.9(2) . . ?
C5 C17 C18 112.15(19) . . ?
C19 C18 C23 118.0(2) . . ?
C19 C18 C17 118.8(2) . . ?
C23 C18 C17 123.1(2) . . ?
C18 C19 C20 123.0(2) . . ?
C21 C20 C19 116.5(2) . . ?
C21 C20 C24 122.5(2) . . ?
C19 C20 C24 121.0(2) . . ?
C20 C21 C22 122.9(2) . . ?
C21 C22 C23 118.2(2) . . ?
C21 C22 C34 119.9(2) . . ?
C23 C22 C34 121.9(2) . . ?
O4 C23 C22 118.8(2) . . ?
O4 C23 C18 120.5(2) . . ?
C22 C23 C18 120.6(2) . . ?
C26 C24 C27 110.5(3) . . ?
C26 C24 C20 108.6(2) . . ?
C27 C24 C20 112.7(2) . . ?
C26 C24 C25 103.6(3) . . ?
C27 C24 C25 110.1(2) . . ?
C20 C24 C25 111.0(2) . . ?
C24 C27 C28 124.6(3) . . ?
C31 C28 C30 110.1(3) . . ?
C31 C28 C29 112.2(4) . . ?
C30 C28 C29 103.8(3) . . ?
C31 C28 C27 112.7(3) . . ?
C30 C28 C27 103.4(3) . . ?
C29 C28 C27 113.9(3) . . ?
O4 C32 C33 112.0(2) . . ?
O6 C33 O5 124.7(3) . . ?
O6 C33 C32 124.7(3) . . ?
O5 C33 C32 110.6(3) . . ?
C22 C34 C35 112.7(2) . . ?
C36 C35 C40 117.3(2) . . ?
C36 C35 C34 119.7(2) . . ?
C40 C35 C34 123.0(2) . . ?
C35 C36 C37 123.2(2) . . ?
C38 C37 C36 116.9(2) . . ?
C38 C37 C41 123.1(2) . . ?
C36 C37 C41 120.0(2) . . ?
C37 C38 C39 122.6(2) . . ?
C40 C39 C38 118.0(2) . . ?
C40 C39 C51 121.8(2) . . ?
C38 C39 C51 120.1(2) . . ?
C39 C40 O7 118.3(2) . . ?
C39 C40 C35 121.7(2) . . ?
O7 C40 C35 120.0(2) . . ?
C37 C41 C43 111.8(2) . . ?
C37 C41 C42 107.6(2) . . ?
C43 C41 C42 106.6(2) . . ?
C37 C41 C44 112.2(2) . . ?
C43 C41 C44 112.4(2) . . ?
C42 C41 C44 105.9(2) . . ?
C45 C44 C41 124.8(2) . . ?
C48 C45 C47 109.2(3) . . ?
C48 C45 C46 107.0(3) . . ?
C47 C45 C46 108.4(3) . . ?
C48 C45 C44 112.8(3) . . ?
C47 C45 C44 113.3(2) . . ?
C46 C45 C44 105.7(2) . . ?
O7 C49 C50 113.6(2) . . ?
O9 C50 O8 125.1(3) . . ?
O9 C50 C49 127.0(3) . . ?
O8 C50 C49 107.9(3) . . ?
C39 C51 C52 109.83(18) . . ?
C53 C52 C57 117.9(2) . . ?
C53 C52 C51 119.4(2) . . ?
C57 C52 C51 122.6(2) . . ?
C54 C53 C52 122.8(2) . . ?
C55 C54 C53 116.7(2) . . ?
C55 C54 C58 120.5(2) . . ?
C53 C54 C58 122.7(2) . . ?
C56 C55 C54 123.1(2) . . ?
C55 C56 C57 118.0(2) . . ?
C55 C56 C68 120.3(2) . . ?
C57 C56 C68 121.7(2) . . ?
O10 C57 C56 118.4(2) . . ?
O10 C57 C52 120.5(2) . . ?
C56 C57 C52 121.1(2) . . ?
C60 C58 C54 111.9(2) . . ?
C60 C58 C59 106.6(2) . . ?
C54 C58 C59 107.2(2) . . ?
C60 C58 C61 112.2(2) . . ?
C54 C58 C61 112.3(2) . . ?
C59 C58 C61 106.1(2) . . ?
C58 C61 C62 123.6(2) . . ?
C65 C62 C64 110.0(3) . . ?
C65 C62 C63 107.5(3) . . ?
C64 C62 C63 107.8(3) . . ?
C65 C62 C61 112.6(2) . . ?
C64 C62 C61 112.6(3) . . ?
C63 C62 C61 106.0(2) . . ?
O10 C66 C67 111.8(2) . . ?
O12 C67 O11 125.0(2) . . ?
O12 C67 C66 124.7(2) . . ?
O11 C67 C66 110.3(2) . . ?
C56 C68 C1 111.72(18) . . ?
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
O1 C6 1.398(3) . ?
O1 C15 1.423(3) . ?
O2 C16 1.306(3) . ?
O3 C16 1.202(3) . ?
O4 C23 1.390(3) . ?
O4 C32 1.422(3) . ?
O5 C33 1.304(3) . ?
O6 C33 1.203(4) . ?
O7 C40 1.395(3) . ?
O7 C49 1.429(3) . ?
O8 C50 1.328(4) . ?
O9 C50 1.194(4) . ?
O10 C57 1.393(3) . ?
O10 C66 1.421(3) . ?
O11 C67 1.308(3) . ?
O12 C67 1.208(3) . ?
C1 C6 1.386(3) . ?
C1 C2 1.396(3) . ?
C1 C68 1.523(3) . ?
C2 C3 1.390(3) . ?
C3 C4 1.398(3) . ?
C3 C7 1.536(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.399(3) . ?
C5 C17 1.519(3) . ?
C7 C9 1.539(4) . ?
C7 C8 1.541(4) . ?
C7 C10 1.553(4) . ?
C10 C11 1.543(4) . ?
C11 C12 1.530(5) . ?
C11 C13 1.530(5) . ?
C11 C14 1.541(5) . ?
C15 C16 1.502(4) . ?
C17 C18 1.522(3) . ?
C18 C19 1.391(3) . ?
C18 C23 1.403(3) . ?
C19 C20 1.395(4) . ?
C20 C21 1.389(4) . ?
C20 C24 1.538(4) . ?
C21 C22 1.394(3) . ?
C22 C23 1.397(3) . ?
C22 C34 1.516(3) . ?
C24 C26 1.488(5) . ?
C24 C27 1.519(4) . ?
C24 C25 1.582(5) . ?
C27 C28 1.560(5) . ?
C28 C31 1.502(5) . ?
C28 C30 1.534(5) . ?
C28 C29 1.535(5) . ?
C32 C33 1.522(4) . ?
C34 C35 1.520(3) . ?
C35 C36 1.388(3) . ?
C35 C40 1.406(3) . ?
C36 C37 1.399(3) . ?
C37 C38 1.387(3) . ?
C37 C41 1.536(3) . ?
C38 C39 1.397(3) . ?
C39 C40 1.389(3) . ?
C39 C51 1.520(3) . ?
C41 C43 1.540(4) . ?
C41 C42 1.543(4) . ?
C41 C44 1.556(4) . ?
C44 C45 1.543(4) . ?
C45 C48 1.532(4) . ?
C45 C47 1.532(4) . ?
C45 C46 1.536(4) . ?
C49 C50 1.504(4) . ?
C51 C52 1.522(3) . ?
C52 C53 1.395(3) . ?
C52 C57 1.399(3) . ?
C53 C54 1.391(3) . ?
C54 C55 1.390(3) . ?
C54 C58 1.541(3) . ?
C55 C56 1.390(3) . ?
C56 C57 1.396(3) . ?
C56 C68 1.514(3) . ?
C58 C60 1.531(4) . ?
C58 C59 1.548(4) . ?
C58 C61 1.548(4) . ?
C61 C62 1.551(4) . ?
C62 C65 1.516(4) . ?
C62 C64 1.527(4) . ?
C62 C63 1.542(4) . ?
C66 C67 1.506(4) . ?
O13 C69 1.418(4) . ?
O14 C70 1.422(5) . ?
O15 C71 1.395(5) . ?
O16 C72 1.380(5) . ?
O17 C73 1.443(7) . ?
