#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:18:18 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180132 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/30/7103037.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_7103037
loop_
_publ_author_name
'Lhoták, Pavel'
'Bílá, Alexandra'
'Budka, Jan'
'Pojarová, Michaela'
'Stibor, Ivan'
_publ_section_title
;
 Simple synthesis of calix[4]arenes in a 1,2-alternate conformation.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1662
_journal_page_last               1664
_journal_paper_doi               10.1039/b718278c
_journal_year                    2008
_chemical_formula_sum            'C64 H77 O4'
_chemical_formula_weight         910.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.46(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.940(7)
_cell_length_b                   20.167(9)
_cell_length_c                   19.074(7)
_cell_measurement_reflns_used    7904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.6581
_cell_measurement_theta_min      3.7810
_cell_volume                     5511(4)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84230
_diffrn_reflns_theta_full        77.70
_diffrn_reflns_theta_max         77.70
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         11474
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0807
_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)+(0.1408P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2439
_reflns_number_gt                5307
_reflns_number_total             11474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718278c.txt
_cod_data_source_block           final_used
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7103037
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C1 C 0.17115(16) 0.53158(10) 0.63665(12) 0.0478(6) Uani 1 1 d . A 1
C2 C 0.11110(18) 0.53794(11) 0.55808(12) 0.0559(7) Uani 1 1 d . A 1
H2A H 0.1403 0.5120 0.5263 0.067 Uiso 1 1 calc R A 1
H2B H 0.0492 0.5182 0.5540 0.067 Uiso 1 1 calc R A 1
C3 C 0.09735(17) 0.60868(11) 0.53019(11) 0.0502(6) Uani 1 1 d . A 1
C4 C 0.00893(17) 0.63668(12) 0.50865(12) 0.0548(7) Uani 1 1 d . A 1
H4 H -0.0433 0.6096 0.5081 0.066 Uiso 1 1 calc R A 1
C5 C -0.00648(17) 0.70273(12) 0.48784(12) 0.0547(7) Uani 1 1 d . A 1
C6 C 0.07327(18) 0.74097(12) 0.49442(12) 0.0569(7) Uani 1 1 d . A 1
H6 H 0.0656 0.7870 0.4839 0.068 Uiso 1 1 calc R A 1
C7 C 0.16324(17) 0.71538(11) 0.51553(11) 0.0497(6) Uani 1 1 d . A 1
C8 C 0.24671(19) 0.75990(12) 0.52481(13) 0.0611(7) Uani 1 1 d . A 1
H8A H 0.2434 0.7811 0.4773 0.073 Uiso 1 1 calc R A 1
H8B H 0.3041 0.7326 0.5391 0.073 Uiso 1 1 calc R A 1
C9 C 0.25293(17) 0.81352(12) 0.58199(12) 0.0541(6) Uani 1 1 d . A 1
C10 C 0.22824(18) 0.87859(12) 0.56073(13) 0.0641(8) Uani 1 1 d . A 1
H10 H 0.2097 0.8890 0.5101 0.077 Uiso 1 1 calc R A 1
C11 C 0.22965(18) 0.92880(12) 0.61061(14) 0.0651(8) Uani 1 1 d . A 1
C12 C 0.25665(18) 0.91103(12) 0.68422(14) 0.0629(7) Uani 1 1 d . A 1
H12 H 0.2568 0.9443 0.7195 0.075 Uiso 1 1 calc R A 1
C13 C 0.28336(16) 0.84715(12) 0.70876(12) 0.0513(6) Uani 1 1 d . A 1
C14 C 0.31196(18) 0.83693(12) 0.79088(12) 0.0593(7) Uani 1 1 d . A 1
H14A H 0.3715 0.8610 0.8106 0.071 Uiso 1 1 calc R A 1
H14B H 0.2649 0.8602 0.8095 0.071 Uiso 1 1 calc R A 1
C15 C 0.32504(17) 0.76985(12) 0.82574(12) 0.0521(6) Uani 1 1 d . A 1
C16 C 0.41024(17) 0.75223(12) 0.87412(12) 0.0558(7) Uani 1 1 d . A 1
H16 H 0.4604 0.7830 0.8831 0.067 Uiso 1 1 calc R A 1
C17 C 0.42511(17) 0.69112(13) 0.91014(12) 0.0552(7) Uani 1 1 d . A 1
C18 C 0.35258(16) 0.64711(13) 0.89363(11) 0.0530(6) Uani 1 1 d . A 1
H18 H 0.3613 0.6049 0.9166 0.064 Uiso 1 1 calc R A 1
C19 C 0.26584(16) 0.66169(12) 0.84421(11) 0.0496(6) Uani 1 1 d . A 1
C20 C 0.19072(16) 0.60854(12) 0.82324(12) 0.0526(6) Uani 1 1 d . A 1
H20A H 0.1286 0.6298 0.8055 0.063 Uiso 1 1 calc R A 1
H20B H 0.1914 0.5815 0.8668 0.063 Uiso 1 1 calc R A 1
C21 C 0.20728(16) 0.56377(11) 0.76349(12) 0.0484(6) Uani 1 1 d . A 1
C22 C 0.28355(16) 0.52137(11) 0.77867(12) 0.0528(6) Uani 1 1 d . A 1
H22 H 0.3223 0.5184 0.8276 0.063 Uiso 1 1 calc R A 1
C23 C 0.30552(16) 0.48316(12) 0.72542(12) 0.0534(6) Uani 1 1 d . A 1
C24 C 0.24929(16) 0.49089(11) 0.65424(12) 0.0500(6) Uani 1 1 d . A 1
H24 H 0.2649 0.4674 0.6161 0.060 Uiso 1 1 calc R A 1
C25 C 0.17352(15) 0.64802(11) 0.52998(11) 0.0482(6) Uani 1 1 d D A 1
C26 C 0.28209(16) 0.79906(11) 0.65623(12) 0.0506(6) Uani 1 1 d . A 1
C27 C 0.25224(15) 0.72390(11) 0.81310(10) 0.0450(6) Uani 1 1 d . A 1
C28 C 0.14990(15) 0.56636(10) 0.69247(12) 0.0467(6) Uani 1 1 d . A 1
O1 O 0.2602(3) 0.6178(3) 0.5448(2) 0.0666(4) Uani 0.46 1 d PD A 1
C29 C 0.2689(4) 0.5905(3) 0.4754(3) 0.0666(4) Uani 0.46 1 d PD A 1
H29A H 0.2152 0.5609 0.4540 0.080 Uiso 0.46 1 calc PR A 1
H29B H 0.2668 0.6272 0.4405 0.080 Uiso 0.46 1 calc PR A 1
C30 C 0.3557(3) 0.5533(3) 0.4855(3) 0.0666(4) Uani 0.46 1 d PD A 1
H30A H 0.3596 0.5378 0.4372 0.080 Uiso 0.46 1 calc PR A 1
H30B H 0.3541 0.5137 0.5157 0.080 Uiso 0.46 1 calc PR A 1
C31 C 0.4427(4) 0.5934(3) 0.5218(3) 0.0666(4) Uani 0.46 1 d PD A 1
O1A O 0.2604(4) 0.6186(5) 0.5453(4) 0.0666(4) Uani 0.33 1 d PD B 2
C29A C 0.2923(5) 0.6082(5) 0.4803(4) 0.0666(4) Uani 0.33 1 d PD B 2
H29C H 0.2788 0.6476 0.4481 0.080 Uiso 0.33 1 calc PR B 2
H29D H 0.2611 0.5692 0.4524 0.080 Uiso 0.33 1 calc PR B 2
C30A C 0.3934(5) 0.5973(4) 0.5080(4) 0.0666(4) Uani 0.33 1 d PD B 2
H30C H 0.4215 0.6357 0.5387 0.080 Uiso 0.33 1 calc PR B 2
H30D H 0.4197 0.5962 0.4658 0.080 Uiso 0.33 1 calc PR B 2
C31A C 0.4234(6) 0.5339(4) 0.5529(4) 0.0666(4) Uani 0.33 1 d PD B 2
O1B O 0.2601(6) 0.6187(9) 0.5460(6) 0.0666(4) Uani 0.21 1 d PD C 3
C29B C 0.3025(7) 0.6094(7) 0.4870(6) 0.0666(4) Uani 0.21 1 d PD C 3
H29E H 0.3277 0.6518 0.4747 0.080 Uiso 0.21 1 calc PR C 3
H29F H 0.2560 0.5923 0.4428 0.080 Uiso 0.21 1 calc PR C 3
C30B C 0.3780(7) 0.5611(6) 0.5140(5) 0.0666(4) Uani 0.21 1 d PD C 3
H30E H 0.3533 0.5188 0.5271 0.080 Uiso 0.21 1 calc PR C 3
H30F H 0.4254 0.5785 0.5575 0.080 Uiso 0.21 1 calc PR C 3
C31B C 0.4195(8) 0.5515(6) 0.4504(5) 0.0666(4) Uani 0.21 1 d PD C 3
O2 O 0.30784(10) 0.73397(7) 0.67679(8) 0.0491(4) Uani 1 1 d . A 1
C32 C 0.40513(17) 0.72241(13) 0.69018(13) 0.0597(7) Uani 1 1 d . A 1
H32A H 0.4407 0.7530 0.7286 0.072 Uiso 1 1 calc R A 1
H32B H 0.4236 0.7309 0.6451 0.072 Uiso 1 1 calc R A 1
C33 C 0.42709(17) 0.65232(13) 0.71411(14) 0.0615(7) Uani 1 1 d . A 1
H33A H 0.3873 0.6220 0.6775 0.074 Uiso 1 1 calc R A 1
H33B H 0.4132 0.6450 0.7613 0.074 Uiso 1 1 calc R A 1
C34 C 0.5294(2) 0.63689(18) 0.72275(19) 0.0988(11) Uani 1 1 d . A 1
H34A H 0.5416 0.6396 0.6750 0.119 Uiso 1 1 calc R A 1
H34B H 0.5437 0.5921 0.7426 0.119 Uiso 1 1 calc R A 1
H34C H 0.5687 0.6690 0.7562 0.119 Uiso 1 1 calc R A 1
O3 O 0.16611(11) 0.74404(8) 0.76835(8) 0.0530(4) Uani 1 1 d . A 1
C35 C 0.11168(17) 0.77524(13) 0.80999(13) 0.0599(7) Uani 1 1 d . A 1
H35A H 0.1539 0.7966 0.8537 0.072 Uiso 1 1 calc R A 1
H35B H 0.0748 0.7412 0.8269 0.072 Uiso 1 1 calc R A 1
C36 C 0.04755(17) 0.82592(11) 0.76606(12) 0.0524(6) Uani 1 1 d . A 1
C37 C 0.04091(18) 0.83953(13) 0.69421(13) 0.0613(7) Uani 1 1 d . A 1
H37 H 0.0794 0.8167 0.6702 0.074 Uiso 1 1 calc R A 1
C38 C -0.0225(2) 0.88698(14) 0.65656(15) 0.0741(9) Uani 1 1 d . A 1
H38 H -0.0251 0.8972 0.6074 0.089 Uiso 1 1 calc R A 1
C39 C -0.0805(2) 0.91884(14) 0.68856(16) 0.0756(9) Uani 1 1 d . A 1
H39 H -0.1247 0.9500 0.6616 0.091 Uiso 1 1 calc R A 1
C40 C -0.0745(2) 0.90551(13) 0.76098(16) 0.0749(8) Uani 1 1 d . A 1
H40 H -0.1153 0.9272 0.7838 0.090 Uiso 1 1 calc R A 1
C41 C -0.00959(18) 0.86097(12) 0.80001(14) 0.0613(7) Uani 1 1 d . A 1
H41 H -0.0035 0.8539 0.8504 0.074 Uiso 1 1 calc R A 1
O4 O 0.06867(10) 0.60371(8) 0.67684(8) 0.0544(4) Uani 1 1 d . A 1
C42 C -0.00817(17) 0.56638(13) 0.68539(17) 0.0710(8) Uani 1 1 d . A 1
H42A H 0.0092 0.5447 0.7339 0.085 Uiso 1 1 calc R A 1
H42B H -0.0246 0.5314 0.6475 0.085 Uiso 1 1 calc R A 1
C43 C -0.09085(18) 0.61092(14) 0.67860(15) 0.0675(8) Uani 1 1 d D A 1
C44 C -0.1771(2) 0.58279(19) 0.6634(2) 0.1143(14) Uani 1 1 d D A 1
H44 H -0.1838 0.5362 0.6569 0.137 Uiso 1 1 calc R A 1
C45 C -0.2556(3) 0.6221(2) 0.6574(3) 0.1325(15) Uani 1 1 d DU A 1
H45 H -0.3160 0.6028 0.6443 0.159 Uiso 1 1 calc R A 1
C46 C -0.2449(2) 0.68912(19) 0.6705(2) 0.1064(12) Uani 1 1 d D A 1
H46 H -0.2976 0.7155 0.6706 0.128 Uiso 1 1 calc R A 1
C47 C -0.1581(2) 0.71816(17) 0.68359(18) 0.0898(10) Uani 1 1 d D A 1
H47 H -0.1512 0.7648 0.6899 0.108 Uiso 1 1 calc R A 1
C48 C -0.0810(2) 0.67849(15) 0.68743(16) 0.0779(9) Uani 1 1 d D A 1
H48 H -0.0210 0.6981 0.6962 0.093 Uiso 1 1 calc R A 1
C49 C -0.1057(4) 0.7320(2) 0.4633(3) 0.0758(6) Uani 0.66 1 d PD A 1
C50 C -0.1815(3) 0.6827(2) 0.4676(2) 0.0758(6) Uani 0.66 1 d PD A 1
H50A H -0.1683 0.6656 0.5176 0.091 Uiso 0.66 1 calc PR A 1
H50B H -0.1826 0.6458 0.4338 0.091 Uiso 0.66 1 calc PR A 1
H50C H -0.2423 0.7050 0.4541 0.091 Uiso 0.66 1 calc PR A 1
C51 C -0.1287(3) 0.7544(2) 0.3816(2) 0.0758(6) Uani 0.66 1 d PD A 1
H51A H -0.1287 0.7156 0.3506 0.091 Uiso 0.66 1 calc PR A 1
H51B H -0.0816 0.7862 0.3761 0.091 Uiso 0.66 1 calc PR A 1
H51C H -0.1904 0.7754 0.3669 0.091 Uiso 0.66 1 calc PR A 1
C52 C -0.1047(3) 0.7906(2) 0.5144(2) 0.0758(6) Uani 0.66 1 d PD A 1
H52A H -0.1649 0.8137 0.4990 0.091 Uiso 0.66 1 calc PR A 1
H52B H -0.0546 0.8213 0.5125 0.091 Uiso 0.66 1 calc PR A 1
H52C H -0.0941 0.7744 0.5645 0.091 Uiso 0.66 1 calc PR A 1
C49A C -0.0996(7) 0.7355(5) 0.4581(5) 0.0758(6) Uani 0.34 1 d PD D 2
C50A C -0.1772(6) 0.6868(4) 0.4295(5) 0.0758(6) Uani 0.34 1 d PD D 2
H50D H -0.1786 0.6551 0.4682 0.091 Uiso 0.34 1 calc PR D 2
H50E H -0.1668 0.6629 0.3878 0.091 Uiso 0.34 1 calc PR D 2
H50F H -0.2368 0.7105 0.4140 0.091 Uiso 0.34 1 calc PR D 2
C51A C -0.0968(6) 0.7807(4) 0.3881(4) 0.0758(6) Uani 0.34 1 d PD D 2
H51D H -0.0869 0.7521 0.3494 0.091 Uiso 0.34 1 calc PR D 2
H51E H -0.0457 0.8128 0.4028 0.091 Uiso 0.34 1 calc PR D 2
H51F H -0.1562 0.8043 0.3698 0.091 Uiso 0.34 1 calc PR D 2
C52A C -0.1277(6) 0.7904(5) 0.5007(5) 0.0758(6) Uani 0.34 1 d PD D 2
H52D H -0.1926 0.8030 0.4770 0.091 Uiso 0.34 1 calc PR D 2
H52E H -0.0871 0.8288 0.5022 0.091 Uiso 0.34 1 calc PR D 2
H52F H -0.1219 0.7752 0.5506 0.091 Uiso 0.34 1 calc PR D 2
C53 C 0.1997(3) 1.0026(2) 0.5902(3) 0.0821(7) Uani 0.67 1 d PD A 1
C54 C 0.1885(3) 1.0141(2) 0.5085(2) 0.0821(7) Uani 0.67 1 d PD A 1
H54A H 0.1417 0.9834 0.4794 0.099 Uiso 0.67 1 calc PR A 1
H54B H 0.2484 1.0064 0.4984 0.099 Uiso 0.67 1 calc PR A 1
H54C H 0.1684 1.0599 0.4956 0.099 Uiso 0.67 1 calc PR A 1
C55 C 0.1095(3) 1.0202(2) 0.6068(2) 0.0821(7) Uani 0.67 1 d PD A 1
H55A H 0.0969 1.0676 0.5981 0.099 Uiso 0.67 1 calc PR A 1
H55B H 0.1148 1.0098 0.6580 0.099 Uiso 0.67 1 calc PR A 1
H55C H 0.0583 0.9944 0.5749 0.099 Uiso 0.67 1 calc PR A 1
C56 C 0.2791(3) 1.0476(2) 0.6324(3) 0.0821(7) Uani 0.67 1 d PD A 1
H56A H 0.2655 1.0935 0.6160 0.099 Uiso 0.67 1 calc PR A 1
H56B H 0.3376 1.0334 0.6234 0.099 Uiso 0.67 1 calc PR A 1
H56C H 0.2850 1.0447 0.6848 0.099 Uiso 0.67 1 calc PR A 1
C53A C 0.2125(7) 0.9964(5) 0.5811(5) 0.0821(7) Uani 0.33 1 d PD E 2
C54A C 0.2781(6) 1.0131(4) 0.5302(5) 0.0821(7) Uani 0.33 1 d PD E 2
H54D H 0.2552 0.9896 0.4835 0.099 Uiso 0.33 1 calc PR E 2
H54E H 0.3421 0.9989 0.5546 0.099 Uiso 0.33 1 calc PR E 2
H54F H 0.2773 1.0609 0.5212 0.099 Uiso 0.33 1 calc PR E 2
C55A C 0.1155(6) 0.9987(4) 0.5327(5) 0.0821(7) Uani 0.33 1 d PD E 2
H55D H 0.0717 0.9933 0.5620 0.099 Uiso 0.33 1 calc PR E 2
H55E H 0.1062 0.9627 0.4967 0.099 Uiso 0.33 1 calc PR E 2
H55F H 0.1044 1.0414 0.5072 0.099 Uiso 0.33 1 calc PR E 2
C56A C 0.2375(7) 1.0464(4) 0.6411(5) 0.0821(7) Uani 0.33 1 d PD E 2
H56D H 0.2499 1.0891 0.6213 0.099 Uiso 0.33 1 calc PR E 2
H56E H 0.2935 1.0317 0.6786 0.099 Uiso 0.33 1 calc PR E 2
H56F H 0.1857 1.0512 0.6627 0.099 Uiso 0.33 1 calc PR E 2
C57 C 0.5176(4) 0.6740(3) 0.9688(3) 0.0760(4) Uani 0.56 1 d PD A 1
C58 C 0.5102(4) 0.6984(3) 1.0437(3) 0.0760(4) Uani 0.56 1 d PD A 1
H58A H 0.5689 0.6892 1.0813 0.091 Uiso 0.56 1 calc PR A 1
H58B H 0.4589 0.6752 1.0559 0.091 Uiso 0.56 1 calc PR A 1
H58C H 0.4981 0.7462 1.0414 0.091 Uiso 0.56 1 calc PR A 1
C59 C 0.6010(3) 0.7071(3) 0.9535(3) 0.0760(4) Uani 0.56 1 d PD A 1
H59A H 0.5990 0.7549 0.9622 0.091 Uiso 0.56 1 calc PR A 1
H59B H 0.5996 0.6992 0.9025 0.091 Uiso 0.56 1 calc PR A 1
H59C H 0.6586 0.6885 0.9860 0.091 Uiso 0.56 1 calc PR A 1
C60 C 0.5397(4) 0.5984(2) 0.9771(3) 0.0760(4) Uani 0.56 1 d PD A 1
H60A H 0.5973 0.5915 1.0166 0.091 Uiso 0.56 1 calc PR A 1
H60B H 0.5477 0.5811 0.9312 0.091 Uiso 0.56 1 calc PR A 1
H60C H 0.4881 0.5752 0.9887 0.091 Uiso 0.56 1 calc PR A 1
C57A C 0.5187(6) 0.6771(4) 0.9647(4) 0.0760(4) Uani 0.44 1 d PD F 2
C58A C 0.5432(5) 0.7293(3) 1.0240(3) 0.0760(4) Uani 0.44 1 d PD F 2
H58D H 0.5959 0.7139 1.0641 0.091 Uiso 0.44 1 calc PR F 2
H58E H 0.4893 0.7374 1.0424 0.091 Uiso 0.44 1 calc PR F 2
H58F H 0.5604 0.7706 1.0039 0.091 Uiso 0.44 1 calc PR F 2
C59A C 0.5931(4) 0.6785(3) 0.9219(3) 0.0760(4) Uani 0.44 1 d PD F 2
H59D H 0.6058 0.7246 0.9114 0.091 Uiso 0.44 1 calc PR F 2
H59E H 0.5696 0.6542 0.8759 0.091 Uiso 0.44 1 calc PR F 2
H59F H 0.6507 0.6577 0.9514 0.091 Uiso 0.44 1 calc PR F 2
C60A C 0.5169(5) 0.6082(3) 0.9979(4) 0.0760(4) Uani 0.44 1 d PD F 2
H60D H 0.5792 0.5972 1.0295 0.091 Uiso 0.44 1 calc PR F 2
H60E H 0.4981 0.5753 0.9586 0.091 Uiso 0.44 1 calc PR F 2
H60F H 0.4721 0.6079 1.0268 0.091 Uiso 0.44 1 calc PR F 2
C61 C 0.3816(4) 0.4306(3) 0.7452(3) 0.0760(4) Uani 0.53 1 d PD A 1
C62 C 0.4688(4) 0.4540(3) 0.8021(3) 0.0760(4) Uani 0.53 1 d PD A 1
H62A H 0.4917 0.4947 0.7851 0.091 Uiso 0.53 1 calc PR A 1
H62B H 0.5170 0.4196 0.8099 0.091 Uiso 0.53 1 calc PR A 1
H62C H 0.4541 0.4628 0.8482 0.091 Uiso 0.53 1 calc PR A 1
C63 C 0.3438(4) 0.3700(3) 0.7814(3) 0.0760(4) Uani 0.53 1 d PD A 1
H63A H 0.3263 0.3854 0.8244 0.091 Uiso 0.53 1 calc PR A 1
H63B H 0.3927 0.3362 0.7961 0.091 Uiso 0.53 1 calc PR A 1
H63C H 0.2891 0.3509 0.7459 0.091 Uiso 0.53 1 calc PR A 1
C64 C 0.4082(4) 0.4029(3) 0.6803(3) 0.0760(4) Uani 0.53 1 d PDU A 1
H64A H 0.3557 0.3777 0.6494 0.091 Uiso 0.53 1 calc PR A 1
H64B H 0.4624 0.3736 0.6975 0.091 Uiso 0.53 1 calc PR A 1
H64C H 0.4239 0.4394 0.6520 0.091 Uiso 0.53 1 calc PR A 1
C61A C 0.3911(5) 0.4352(4) 0.7448(4) 0.0760(4) Uani 0.47 1 d PD G 2
C62A C 0.4607(5) 0.4563(4) 0.8183(3) 0.0760(4) Uani 0.47 1 d PD G 2
H62D H 0.5130 0.4251 0.8312 0.091 Uiso 0.47 1 calc PR G 2
H62E H 0.4289 0.4563 0.8568 0.091 Uiso 0.47 1 calc PR G 2
H62F H 0.4842 0.5010 0.8134 0.091 Uiso 0.47 1 calc PR G 2
C63A C 0.3529(4) 0.3655(3) 0.7485(3) 0.0760(4) Uani 0.47 1 d PD G 2
H63D H 0.3103 0.3537 0.7008 0.091 Uiso 0.47 1 calc PR G 2
H63E H 0.3191 0.3642 0.7857 0.091 Uiso 0.47 1 calc PR G 2
H63F H 0.4047 0.3338 0.7613 0.091 Uiso 0.47 1 calc PR G 2
C64A C 0.4407(4) 0.4384(3) 0.6851(3) 0.0760(4) Uani 0.47 1 d PDU G 2
H64D H 0.4679 0.4825 0.6848 0.091 Uiso 0.47 1 calc PR G 2
H64E H 0.3958 0.4297 0.6375 0.091 Uiso 0.47 1 calc PR G 2
H64F H 0.4903 0.4049 0.6947 0.091 Uiso 0.47 1 calc PR G 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'
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
_geom_angle_publ_flag
C28 C1 C24 118.3(2) . . ?
C28 C1 C2 121.1(2) . . ?
C24 C1 C2 120.6(2) . . ?
C3 C2 C1 114.15(18) . . ?
C4 C3 C25 118.6(2) . . ?
C4 C3 C2 120.7(2) . . ?
C25 C3 C2 120.6(2) . . ?
C3 C4 C5 122.8(2) . . ?
C4 C5 C6 115.8(2) . . ?
C4 C5 C49 121.4(3) . . ?
C6 C5 C49 122.7(3) . . ?
C7 C6 C5 123.5(2) . . ?
C25 C7 C6 117.7(2) . . ?
C25 C7 C8 121.3(2) . . ?
C6 C7 C8 120.9(2) . . ?
C7 C8 C9 112.9(2) . . ?
C26 C9 C10 118.4(2) . . ?
C26 C9 C8 121.3(2) . . ?
C10 C9 C8 120.3(2) . . ?
C11 C10 C9 122.5(2) . . ?
C10 C11 C12 116.6(2) . . ?
C10 C11 C53 125.1(3) . . ?
C12 C11 C53 118.3(3) . . ?
C13 C12 C11 123.5(2) . . ?
C12 C13 C26 117.4(2) . . ?
C12 C13 C14 116.4(2) . . ?
C26 C13 C14 126.3(2) . . ?
C15 C14 C13 123.0(2) . . ?
C16 C15 C27 117.8(2) . . ?
C16 C15 C14 120.4(2) . . ?
C27 C15 C14 121.7(2) . . ?
C15 C16 C17 122.7(2) . . ?
C18 C17 C16 117.0(2) . . ?
C18 C17 C57 120.6(3) . . ?
C16 C17 C57 122.4(3) . . ?
C17 C18 C19 122.7(2) . . ?
C27 C19 C18 118.4(2) . . ?
C27 C19 C20 121.4(2) . . ?
C18 C19 C20 120.1(2) . . ?
C19 C20 C21 110.43(19) . . ?
C28 C21 C22 118.2(2) . . ?
C28 C21 C20 121.4(2) . . ?
C22 C21 C20 120.3(2) . . ?
C23 C22 C21 122.7(2) . . ?
C22 C23 C24 116.8(2) . . ?
C22 C23 C61 121.4(3) . . ?
C24 C23 C61 121.5(3) . . ?
C23 C24 C1 122.5(2) . . ?
C7 C25 O1 121.0(3) . . ?
C7 C25 C3 121.1(2) . . ?
O1 C25 C3 117.9(3) . . ?
C9 C26 C13 121.6(2) . . ?
C9 C26 O2 117.8(2) . . ?
C13 C26 O2 120.55(19) . . ?
C19 C27 O3 121.9(2) . . ?
C19 C27 C15 121.1(2) . . ?
O3 C27 C15 116.9(2) . . ?
C21 C28 C1 121.3(2) . . ?
C21 C28 O4 119.5(2) . . ?
C1 C28 O4 119.14(19) . . ?
C25 O1 C29 107.2(3) . . ?
C30 C29 O1 111.9(4) . . ?
C29 C30 C31 113.5(5) . . ?
O1A C29A C30A 105.4(6) . . ?
C29A C30A C31A 115.7(7) . . ?
O1B C29B C30B 105.9(9) . . ?
C29B C30B C31B 104.5(8) . . ?
C26 O2 C32 113.08(17) . . ?
O2 C32 C33 109.6(2) . . ?
C32 C33 C34 110.7(2) . . ?
C27 O3 C35 111.11(16) . . ?
O3 C35 C36 111.5(2) . . ?
C37 C36 C41 118.6(2) . . ?
C37 C36 C35 123.5(2) . . ?
C41 C36 C35 117.8(2) . . ?
C36 C37 C38 119.8(3) . . ?
C39 C38 C37 121.4(3) . . ?
C38 C39 C40 119.2(3) . . ?
C41 C40 C39 120.2(3) . . ?
C40 C41 C36 120.5(3) . . ?
C28 O4 C42 111.96(18) . . ?
O4 C42 C43 110.2(2) . . ?
C44 C43 C48 120.0(3) . . ?
C44 C43 C42 118.3(3) . . ?
C48 C43 C42 121.7(2) . . ?
C43 C44 C45 120.3(3) . . ?
C46 C45 C44 119.5(3) . . ?
C45 C46 C47 120.3(3) . . ?
C46 C47 C48 119.2(3) . . ?
C43 C48 C47 120.4(3) . . ?
C50 C49 C52 110.0(4) . . ?
C50 C49 C5 113.5(4) . . ?
C52 C49 C5 105.6(3) . . ?
C50 C49 C51 106.5(4) . . ?
C52 C49 C51 111.8(4) . . ?
C5 C49 C51 109.5(4) . . ?
C50A C49A C52A 111.9(9) . . ?
C50A C49A C51A 105.4(7) . . ?
C52A C49A C51A 96.2(7) . . ?
C55 C53 C56 110.9(4) . . ?
C55 C53 C54 109.2(4) . . ?
C56 C53 C54 106.8(4) . . ?
C55 C53 C11 112.3(4) . . ?
C56 C53 C11 107.9(3) . . ?
C54 C53 C11 109.6(4) . . ?
C55A C53A C56A 116.5(8) . . ?
C55A C53A C54A 105.9(8) . . ?
C56A C53A C54A 105.1(8) . . ?
C59 C57 C58 108.5(5) . . ?
C59 C57 C17 112.2(4) . . ?
C58 C57 C17 108.3(4) . . ?
C59 C57 C60 106.7(5) . . ?
C58 C57 C60 106.6(4) . . ?
C17 C57 C60 114.2(4) . . ?
C58A C57A C60A 110.6(6) . . ?
C58A C57A C59A 108.8(6) . . ?
C60A C57A C59A 109.4(6) . . ?
C64 C61 C62 109.3(5) . . ?
C64 C61 C23 114.0(4) . . ?
C62 C61 C23 113.0(5) . . ?
C64 C61 C63 106.3(5) . . ?
C62 C61 C63 105.5(5) . . ?
C23 C61 C63 108.2(5) . . ?
C63A C61A C64A 109.9(6) . . ?
C63A C61A C62A 112.1(6) . . ?
C64A C61A C62A 108.6(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C28 1.385(3) . ?
C1 C24 1.388(3) . ?
C1 C2 1.519(3) . ?
C2 C3 1.516(3) . ?
C3 C4 1.387(3) . ?
C3 C25 1.388(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.395(4) . ?
C5 C49 1.539(6) . ?
C6 C7 1.389(3) . ?
C7 C25 1.386(3) . ?
C7 C8 1.506(3) . ?
C8 C9 1.520(3) . ?
C9 C26 1.390(3) . ?
C9 C10 1.392(3) . ?
C10 C11 1.385(4) . ?
C11 C12 1.394(3) . ?
C11 C53 1.571(5) . ?
C12 C13 1.390(3) . ?
C13 C26 1.391(3) . ?
C13 C14 1.516(3) . ?
C14 C15 1.496(3) . ?
C15 C16 1.390(3) . ?
C15 C27 1.397(3) . ?
C16 C17 1.398(3) . ?
C17 C18 1.367(3) . ?
C17 C57 1.550(6) . ?
C18 C19 1.401(3) . ?
C19 C27 1.378(3) . ?
C19 C20 1.521(3) . ?
C20 C21 1.528(3) . ?
C21 C28 1.384(3) . ?
C21 C22 1.388(3) . ?
C22 C23 1.386(3) . ?
C23 C24 1.388(3) . ?
C23 C61 1.521(7) . ?
C25 O1 1.386(5) . ?
C26 O2 1.393(3) . ?
C27 O3 1.388(3) . ?
C28 O4 1.387(3) . ?
O1 C29 1.473(6) . ?
C29 C30 1.463(6) . ?
C30 C31 1.521(6) . ?
O1A C29A 1.463(7) . ?
C29A C30A 1.469(7) . ?
C30A C31A 1.533(7) . ?
O1B C29B 1.451(9) . ?
C29B C30B 1.469(9) . ?
C30B C31B 1.523(9) . ?
O2 C32 1.422(3) . ?
C32 C33 1.493(3) . ?
C33 C34 1.522(4) . ?
O3 C35 1.433(3) . ?
C35 C36 1.486(3) . ?
C36 C37 1.373(3) . ?
C36 C41 1.400(4) . ?
C37 C38 1.394(4) . ?
C38 C39 1.355(4) . ?
C39 C40 1.385(4) . ?
C40 C41 1.376(4) . ?
O4 C42 1.420(3) . ?
C42 C43 1.503(4) . ?
C43 C44 1.362(4) . ?
C43 C48 1.376(4) . ?
C44 C45 1.393(5) . ?
C45 C46 1.376(5) . ?
C46 C47 1.380(4) . ?
C47 C48 1.387(4) . ?
C49 C50 1.527(6) . ?
C49 C52 1.530(6) . ?
C49 C51 1.566(6) . ?
C49A C50A 1.500(11) . ?
C49A C52A 1.503(11) . ?
C49A C51A 1.626(11) . ?
C53 C55 1.510(6) . ?
C53 C56 1.528(6) . ?
C53 C54 1.538(6) . ?
C53A C55A 1.483(11) . ?
C53A C56A 1.490(11) . ?
C53A C54A 1.600(12) . ?
C57 C59 1.513(8) . ?
C57 C58 1.543(7) . ?
C57 C60 1.559(7) . ?
C57A C58A 1.512(9) . ?
C57A C60A 1.531(9) . ?
C57A C59A 1.555(10) . ?
C61 C64 1.510(8) . ?
C61 C62 1.516(7) . ?
C61 C63 1.583(8) . ?
C61A C63A 1.526(9) . ?
C61A C64A 1.526(9) . ?
C61A C62A 1.550(8) . ?
