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#                                CCDC 
# 
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#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_gen9
_database_code_depnum_ccdc_archive 'CCDC 603037'

_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common 't-bu-calix[4]arene menthol'
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C98 H132 O9'
_chemical_formula_weight 1454.04

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'

_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a 12.6609(10)
_cell_length_b 12.8921(10)
_cell_length_c 14.5868(12)
_cell_angle_alpha 112.0560(10)
_cell_angle_beta 103.324(2)
_cell_angle_gamma 90.492(2)
_cell_volume 2135.3(3)
_cell_formula_units_Z 1
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?

_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.131
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 792
_exptl_absorpt_coefficient_mu 0.070
_exptl_absorpt_correction_type multiscan
_exptl_absorpt_correction_T_min 0.9657
_exptl_absorpt_correction_T_max 0.9895
_exptl_absorpt_process_details sadabs

_exptl_special_details
;
?
;

_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 25418
_diffrn_reflns_av_R_equivalents 0.0311
_diffrn_reflns_av_sigmaI/netI 0.0372
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 1.66
_diffrn_reflns_theta_max 28.75
_reflns_number_total 10936
_reflns_number_gt 8114
_reflns_threshold_expression >2sigma(I)

_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?

_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+2.5532P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10936
_refine_ls_number_parameters 551
_refine_ls_number_restraints 71
_refine_ls_R_factor_all 0.0991
_refine_ls_R_factor_gt 0.0764
_refine_ls_wR_factor_ref 0.2282
_refine_ls_wR_factor_gt 0.2118
_refine_ls_goodness_of_fit_ref 0.989
_refine_ls_restrained_S_all 0.991
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.17302(13) 0.59715(14) 0.45503(12) 0.0290(3) Uani 1 1 d . . .
H1 H 0.1318 0.6446 0.4449 0.043 Uiso 1 1 calc R . .
O2 O 0.30968(13) 0.85764(14) 0.45682(12) 0.0293(3) Uani 1 1 d . . .
H2 H 0.3485 0.8040 0.4495 0.044 Uiso 1 1 calc R . .
O3 O 0.10675(13) 0.79046(14) 0.44935(12) 0.0294(3) Uani 1 1 d . . .
H3 H 0.1684 0.8152 0.4496 0.044 Uiso 1 1 calc R . .
O4 O 0.37415(13) 0.66751(14) 0.46231(12) 0.0287(3) Uani 1 1 d . . .
H4 H 0.3154 0.6328 0.4576 0.043 Uiso 1 1 calc R . .
C1 C 0.16674(17) 0.58660(17) 0.54505(16) 0.0224(4) Uani 1 1 d . . .
C2 C 0.24947(16) 0.53746(17) 0.59051(17) 0.0239(4) Uani 1 1 d . . .
C3 C 0.24121(17) 0.52338(19) 0.67894(18) 0.0268(4) Uani 1 1 d . . .
H3A H 0.2974 0.4904 0.7107 0.032 Uiso 1 1 calc R . .
C4 C 0.15355(18) 0.55588(19) 0.72240(17) 0.0260(4) Uani 1 1 d . . .
C5 C 0.07277(17) 0.60533(18) 0.67414(17) 0.0246(4) Uani 1 1 d . . .
H5 H 0.0122 0.6281 0.7024 0.030 Uiso 1 1 calc R . .
C6 C 0.07781(16) 0.62245(17) 0.58654(16) 0.0220(4) Uani 1 1 d . . .
C7 C -0.01026(16) 0.68080(18) 0.53988(17) 0.0248(4) Uani 1 1 d . . .
H7A H -0.0801 0.6642 0.5537 0.030 Uiso 1 1 calc R . .
H7B H -0.0205 0.6499 0.4648 0.030 Uiso 1 1 calc R . .
C8 C 0.1418(2) 0.5384(2) 0.8182(2) 0.0346(5) Uani 1 1 d . . .
C9 C 0.2425(3) 0.4964(4) 0.8671(3) 0.0593(9) Uani 1 1 d . . .
H9A H 0.2312 0.4860 0.9274 0.071 Uiso 1 1 calc R . .
H9B H 0.3059 0.5517 0.8875 0.071 Uiso 1 1 calc R . .
H9C H 0.2556 0.4245 0.8178 0.071 Uiso 1 1 calc R . .
C10 C 0.0432(3) 0.4516(3) 0.7884(3) 0.0528(8) Uani 1 1 d . . .
H10A H 0.0558 0.3794 0.7393 0.063 Uiso 1 1 calc R . .
H10B H -0.0226 0.4780 0.7574 0.063 Uiso 1 1 calc R . .
H10C H 0.0334 0.4420 0.8496 0.063 Uiso 1 1 calc R . .
C11 C 0.1224(3) 0.6492(3) 0.8989(2) 0.0536(8) Uani 1 1 d . . .
H11A H 0.1155 0.6367 0.9595 0.064 Uiso 1 1 calc R . .
H11B H 0.0552 0.6758 0.8706 0.064 Uiso 1 1 calc R . .
H11C H 0.1842 0.7059 0.9179 0.064 Uiso 1 1 calc R . .
C12 C 0.07827(16) 0.85852(18) 0.53728(16) 0.0225(4) Uani 1 1 d . A .
C13 C 0.01745(16) 0.80824(18) 0.58179(16) 0.0219(4) Uani 1 1 d . . .
C14 C -0.01485(17) 0.87739(18) 0.66679(17) 0.0243(4) Uani 1 1 d . A .
H14 H -0.0567 0.8440 0.6968 0.029 Uiso 1 1 calc R . .
C15 C 0.01106(17) 0.99423(18) 0.71068(16) 0.0238(4) Uani 1 1 d D . .
C16 C 0.07293(17) 1.04002(18) 0.66450(17) 0.0250(4) Uani 1 1 d . A .
H16 H 0.0920 1.1191 0.6927 0.030 Uiso 1 1 calc R . .
C17 C 0.10785(16) 0.97450(18) 0.57886(17) 0.0236(4) Uani 1 1 d . . .
C18 C 0.17737(17) 1.03030(19) 0.53440(18) 0.0262(4) Uani 1 1 d . A .
H18A H 0.1562 1.1070 0.5454 0.031 Uiso 1 1 calc R . .
H18B H 0.1624 0.9868 0.4598 0.031 Uiso 1 1 calc R . .
C19 C -0.0289(3) 1.0653(2) 0.8039(2) 0.0316(5) Uani 0.93 1 d PD A -1
C20 C 0.0142(3) 1.0258(3) 0.8910(2) 0.0454(7) Uani 0.93 1 d PD A -1
H20A H 0.0941 1.0387 0.9118 0.055 Uiso 0.93 1 calc PR A -1
H20B H -0.0086 0.9453 0.8677 0.055 Uiso 0.93 1 calc PR A -1
H20C H -0.0153 1.0681 0.9493 0.055 Uiso 0.93 1 calc PR A -1
C21 C -0.1540(2) 1.0496(3) 0.7764(3) 0.0456(7) Uani 0.93 1 d PD A -1
H21A H -0.1797 1.0926 0.8369 0.055 Uiso 0.93 1 calc PR A -1
H21B H -0.1792 0.9697 0.7527 0.055 Uiso 0.93 1 calc PR A -1
H21C H -0.1829 1.0767 0.7220 0.055 Uiso 0.93 1 calc PR A -1
C22 C 0.0092(4) 1.1902(3) 0.8411(3) 0.0570(10) Uani 0.93 1 d PD A -1
H22A H -0.0197 1.2329 0.8996 0.068 Uiso 0.93 1 calc PR A -1
H22B H -0.0174 1.2165 0.7858 0.068 Uiso 0.93 1 calc PR A -1
H22C H 0.0892 1.2015 0.8617 0.068 Uiso 0.93 1 calc PR A -1
C19B C -0.025(2) 1.082(3) 0.804(2) 0.0316(5) Uani 0.07 1 d PD A -2
C20B C -0.084(3) 1.021(3) 0.852(2) 0.0454(7) Uani 0.07 1 d PD A -2
H20D H -0.1505 0.9771 0.8023 0.055 Uiso 0.07 1 calc PR A -2
H20E H -0.1031 1.0761 0.9120 0.055 Uiso 0.07 1 calc PR A -2
H20F H -0.0361 0.9703 0.8734 0.055 Uiso 0.07 1 calc PR A -2
C21B C -0.102(3) 1.157(2) 0.768(3) 0.0456(7) Uani 0.07 1 d PD A -2
H21D H -0.0685 1.1886 0.7281 0.055 Uiso 0.07 1 calc PR A -2
H21E H -0.1155 1.2184 0.8269 0.055 Uiso 0.07 1 calc PR A -2
H21F H -0.1710 1.1123 0.7244 0.055 Uiso 0.07 1 calc PR A -2
C22B C 0.075(3) 1.155(2) 0.8841(17) 0.0570(10) Uani 0.07 1 d PD A -2
H22D H 0.1217 1.1072 0.9116 0.068 Uiso 0.07 1 calc PR A -2
H22E H 0.0521 1.2127 0.9395 0.068 Uiso 0.07 1 calc PR A -2
H22F H 0.1165 1.1904 0.8526 0.068 Uiso 0.07 1 calc PR A -2
C23 C 0.36076(17) 0.94938(18) 0.54426(16) 0.0226(4) Uani 1 1 d . A .
C24 C 0.29928(17) 1.03818(18) 0.58200(17) 0.0237(4) Uani 1 1 d . . .
C25 C 0.35170(18) 1.13377(19) 0.66436(17) 0.0254(4) Uani 1 1 d . A .
H25 H 0.3104 1.1944 0.6900 0.030 Uiso 1 1 calc R . .
C26 C 0.46339(17) 1.14499(18) 0.71163(17) 0.0240(4) Uani 1 1 d . . .
C27 C 0.52045(17) 1.05258(18) 0.67346(17) 0.0233(4) Uani 1 1 d . A .
H27 H 0.5959 1.0573 0.7049 0.028 Uiso 1 1 calc R . .
C28 C 0.47119(16) 0.95346(17) 0.59086(16) 0.0209(4) Uani 1 1 d . . .
C29 C 0.53860(17) 0.85624(18) 0.55268(16) 0.0232(4) Uani 1 1 d . A .
H29A H 0.5139 0.8212 0.4772 0.028 Uiso 1 1 calc R . .
H29B H 0.6158 0.8872 0.5707 0.028 Uiso 1 1 calc R . .
C30 C 0.51694(19) 1.2570(2) 0.79765(19) 0.0309(5) Uani 1 1 d . A .
C31 C 0.6394(2) 1.2557(3) 0.8369(3) 0.0511(8) Uani 1 1 d . . .
H31A H 0.6519 1.1948 0.8616 0.061 Uiso 1 1 calc R A .
H31B H 0.6698 1.3279 0.8930 0.061 Uiso 1 1 calc R . .
H31C H 0.6750 1.2435 0.7813 0.061 Uiso 1 1 calc R . .
C32 C 0.5002(2) 1.3517(2) 0.7565(2) 0.0390(6) Uani 1 1 d . . .
H32A H 0.5335 1.4238 0.8112 0.047 Uiso 1 1 calc R A .
H32B H 0.4219 1.3554 0.7326 0.047 Uiso 1 1 calc R . .
H32C H 0.5346 1.3358 0.6996 0.047 Uiso 1 1 calc R . .
C33 C 0.4633(3) 1.2836(2) 0.8867(2) 0.0430(6) Uani 1 1 d . . .
H33A H 0.4716 1.2231 0.9123 0.052 Uiso 1 1 calc R A .
H33B H 0.3855 1.2898 0.8631 0.052 Uiso 1 1 calc R . .
H33C H 0.4983 1.3549 0.9417 0.052 Uiso 1 1 calc R . .
C34 C 0.44930(17) 0.67603(18) 0.55057(16) 0.0229(4) Uani 1 1 d . A .
C35 C 0.53318(16) 0.76468(17) 0.59431(16) 0.0214(4) Uani 1 1 d . . .
C36 C 0.61406(17) 0.76642(18) 0.67885(17) 0.0241(4) Uani 1 1 d . A .
H36 H 0.6717 0.8259 0.7094 0.029 Uiso 1 1 calc R . .
C37 C 0.61365(17) 0.68475(18) 0.72005(17) 0.0241(4) Uani 1 1 d . . .
C38 C 0.52559(17) 0.60069(19) 0.67559(18) 0.0258(4) Uani 1 1 d . A .
H38 H 0.5221 0.5456 0.7038 0.031 Uiso 1 1 calc R . .
C39 C 0.44297(17) 0.59460(17) 0.59186(17) 0.0235(4) Uani 1 1 d . . .
C40 C 0.34840(17) 0.50202(18) 0.54788(18) 0.0259(4) Uani 1 1 d . A .
H40A H 0.3736 0.4361 0.5625 0.031 Uiso 1 1 calc R . .
H40B H 0.3262 0.4785 0.4727 0.031 Uiso 1 1 calc R . .
C41 C 0.70478(19) 0.6816(2) 0.80922(18) 0.0293(5) Uani 1 1 d . A .
C42 C 0.7951(2) 0.7790(3) 0.8481(2) 0.0454(7) Uani 1 1 d . . .
H42A H 0.7642 0.8507 0.8735 0.055 Uiso 1 1 calc R A .
H42B H 0.8269 0.7760 0.7920 0.055 Uiso 1 1 calc R . .
H42C H 0.8519 0.7727 0.9035 0.055 Uiso 1 1 calc R . .
C43 C 0.7567(2) 0.5708(2) 0.7727(2) 0.0414(6) Uani 1 1 d . . .
H43A H 0.8135 0.5673 0.8296 0.050 Uiso 1 1 calc R A .
H43B H 0.7892 0.5672 0.7169 0.050 Uiso 1 1 calc R . .
H43C H 0.7005 0.5071 0.7484 0.050 Uiso 1 1 calc R . .
C44 C 0.6577(2) 0.6870(3) 0.8984(2) 0.0409(6) Uani 1 1 d . . .
H44A H 0.6224 0.7562 0.9212 0.049 Uiso 1 1 calc R A .
H44B H 0.7167 0.6864 0.9550 0.049 Uiso 1 1 calc R . .
H44C H 0.6039 0.6217 0.8761 0.049 Uiso 1 1 calc R . .
O1A O 0.6338(4) 1.0140(5) 0.8999(4) 0.0657(14) Uani 0.50 1 d PD B -2
H1A H 0.6215 0.9697 0.8383 0.079 Uiso 0.50 1 calc PR B -2
C1A C 0.5406(8) 1.0127(10) 0.9344(9) 0.039(3) Uani 0.50 1 d PD B -2
H1A1 H 0.5174 1.0891 0.9434 0.047 Uiso 0.50 1 calc PR B -2
C2A C 0.4469(5) 0.9372(5) 0.8521(4) 0.0488(14) Uani 0.50 1 d PD B -2
H2A1 H 0.4307 0.9654 0.7964 0.059 Uiso 0.50 1 calc PR B -2
H2A2 H 0.4712 0.8614 0.8238 0.059 Uiso 0.50 1 calc PR B -2
C3A C 0.3478(9) 0.9248(12) 0.8785(8) 0.085(6) Uani 0.50 1 d PD B -2
H3A1 H 0.3238 1.0002 0.8846 0.102 Uiso 0.50 1 calc PR B -2
C4A C 0.3536(7) 0.9369(12) 0.9829(6) 0.113(5) Uani 0.50 1 d PD B -2
H4A1 H 0.3591 0.8617 0.9861 0.136 Uiso 0.50 1 calc PR B -2
H4A2 H 0.2841 0.9626 0.9991 0.136 Uiso 0.50 1 calc PR B -2
C5A C 0.4457(9) 1.0162(10) 1.0640(10) 0.043(3) Uani 0.50 1 d PD B -2
H5A1 H 0.4247 1.0938 1.0816 0.051 Uiso 0.50 1 calc PR B -2
H5A2 H 0.4560 0.9991 1.1260 0.051 Uiso 0.50 1 calc PR B -2
C6A C 0.5524(6) 1.0125(11) 1.0357(5) 0.100(4) Uani 0.50 1 d PD B -2
H6A H 0.5697 0.9341 1.0258 0.120 Uiso 0.50 1 calc PR B -2
C7A C 0.6531(7) 1.0834(10) 1.1153(7) 0.061(5) Uani 0.50 1 d PD B -2
H7A1 H 0.7104 1.0878 1.0794 0.073 Uiso 0.50 1 calc PR B -2
C8A C 0.6348(7) 1.1998(6) 1.1773(11) 0.122(5) Uani 0.50 1 d PD B -2
H8A1 H 0.6196 1.2430 1.1338 0.147 Uiso 0.50 1 calc PR B -2
H8A2 H 0.7002 1.2358 1.2329 0.147 Uiso 0.50 1 calc PR B -2
H8A3 H 0.5725 1.1973 1.2060 0.147 Uiso 0.50 1 calc PR B -2
C9A C 0.6955(7) 1.0243(11) 1.1871(11) 0.124(6) Uani 0.50 1 d PD B -2
H9A1 H 0.7640 1.0656 1.2354 0.149 Uiso 0.50 1 calc PR B -2
H9A2 H 0.7085 0.9474 1.1473 0.149 Uiso 0.50 1 calc PR B -2
H9A3 H 0.6414 1.0217 1.2248 0.149 Uiso 0.50 1 calc PR B -2
C10A C 0.2511(5) 0.8554(6) 0.7987(6) 0.0594(18) Uani 0.50 1 d PD B -2
H10D H 0.2671 0.7771 0.7705 0.071 Uiso 0.50 1 calc PR B -2
H10E H 0.2336 0.8839 0.7439 0.071 Uiso 0.50 1 calc PR B -2
H10F H 0.1888 0.8595 0.8287 0.071 Uiso 0.50 1 calc PR B -2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0296(8) 0.0312(8) 0.0250(8) 0.0099(7) 0.0065(6) 0.0028(6)
O2 0.0292(8) 0.0312(8) 0.0264(8) 0.0103(7) 0.0064(6) 0.0020(6)
O3 0.0278(8) 0.0345(9) 0.0260(8) 0.0107(7) 0.0084(6) 0.0022(6)
O4 0.0266(8) 0.0298(8) 0.0272(8) 0.0090(7) 0.0055(6) 0.0003(6)
C1 0.0227(9) 0.0184(9) 0.0226(10) 0.0050(8) 0.0042(8) -0.0023(7)
C2 0.0188(9) 0.0196(9) 0.0293(11) 0.0061(8) 0.0045(8) -0.0009(7)
C3 0.0215(9) 0.0254(11) 0.0320(11) 0.0112(9) 0.0040(8) 0.0026(8)
C4 0.0263(10) 0.0249(10) 0.0269(10) 0.0099(9) 0.0074(8) 0.0028(8)
C5 0.0207(9) 0.0235(10) 0.0287(11) 0.0084(8) 0.0073(8) 0.0030(7)
C6 0.0198(9) 0.0183(9) 0.0238(10) 0.0055(8) 0.0028(7) -0.0011(7)
C7 0.0177(9) 0.0253(10) 0.0293(11) 0.0105(9) 0.0023(8) -0.0007(7)
C8 0.0352(12) 0.0408(14) 0.0342(13) 0.0200(11) 0.0116(10) 0.0096(10)
C9 0.0540(18) 0.098(3) 0.0496(18) 0.0480(19) 0.0238(15) 0.0361(19)
C10 0.0604(19) 0.0544(19) 0.0548(18) 0.0309(16) 0.0195(15) -0.0004(15)
C11 0.074(2) 0.0522(18) 0.0386(15) 0.0173(14) 0.0228(15) 0.0183(16)
C12 0.0180(9) 0.0282(10) 0.0220(10) 0.0117(8) 0.0029(7) 0.0034(7)
C13 0.0158(8) 0.0243(10) 0.0252(10) 0.0118(8) 0.0008(7) 0.0007(7)
C14 0.0202(9) 0.0270(11) 0.0285(11) 0.0144(9) 0.0053(8) 0.0015(8)
C15 0.0224(9) 0.0254(10) 0.0234(10) 0.0103(8) 0.0042(8) 0.0032(8)
C16 0.0216(9) 0.0231(10) 0.0304(11) 0.0113(9) 0.0050(8) 0.0008(8)
C17 0.0171(9) 0.0275(10) 0.0296(10) 0.0161(9) 0.0038(8) 0.0025(7)
C18 0.0226(10) 0.0294(11) 0.0330(11) 0.0185(9) 0.0084(8) 0.0044(8)
C19 0.0386(13) 0.0289(14) 0.0286(11) 0.0093(10) 0.0142(10) 0.0028(10)
C20 0.0599(19) 0.0463(17) 0.0273(13) 0.0115(12) 0.0104(13) 0.0034(14)
C21 0.0411(15) 0.0542(19) 0.0495(18) 0.0202(15) 0.0257(14) 0.0162(14)
C22 0.089(3) 0.0272(15) 0.059(2) 0.0058(14) 0.046(2) 0.0014(15)
C19B 0.0386(13) 0.0289(14) 0.0286(11) 0.0093(10) 0.0142(10) 0.0028(10)
C20B 0.0599(19) 0.0463(17) 0.0273(13) 0.0115(12) 0.0104(13) 0.0034(14)
C21B 0.0411(15) 0.0542(19) 0.0495(18) 0.0202(15) 0.0257(14) 0.0162(14)
C22B 0.089(3) 0.0272(15) 0.059(2) 0.0058(14) 0.046(2) 0.0014(15)
C23 0.0244(10) 0.0241(10) 0.0230(10) 0.0120(8) 0.0078(8) 0.0017(8)
C24 0.0217(9) 0.0275(10) 0.0296(11) 0.0181(9) 0.0092(8) 0.0033(8)
C25 0.0255(10) 0.0244(10) 0.0310(11) 0.0131(9) 0.0118(8) 0.0050(8)
C26 0.0249(10) 0.0245(10) 0.0255(10) 0.0116(8) 0.0090(8) 0.0040(8)
C27 0.0215(9) 0.0243(10) 0.0274(10) 0.0122(8) 0.0085(8) 0.0029(8)
C28 0.0225(9) 0.0221(9) 0.0241(10) 0.0128(8) 0.0104(8) 0.0040(7)
C29 0.0229(9) 0.0233(10) 0.0255(10) 0.0086(8) 0.0114(8) 0.0023(8)
C30 0.0291(11) 0.0266(11) 0.0328(12) 0.0076(9) 0.0065(9) 0.0045(9)
C31 0.0361(14) 0.0367(15) 0.0547(18) -0.0029(13) -0.0021(13) 0.0040(11)
C32 0.0471(15) 0.0264(12) 0.0429(14) 0.0118(11) 0.0132(12) -0.0006(10)
C33 0.0576(17) 0.0407(15) 0.0307(13) 0.0111(11) 0.0159(12) 0.0107(13)
C34 0.0219(9) 0.0230(10) 0.0230(10) 0.0069(8) 0.0080(8) 0.0038(8)
C35 0.0215(9) 0.0197(9) 0.0233(10) 0.0055(8) 0.0110(8) 0.0040(7)
C36 0.0225(9) 0.0224(10) 0.0262(10) 0.0069(8) 0.0086(8) 0.0004(7)
C37 0.0221(9) 0.0248(10) 0.0254(10) 0.0083(8) 0.0084(8) 0.0033(8)
C38 0.0235(10) 0.0247(10) 0.0313(11) 0.0116(9) 0.0097(8) 0.0031(8)
C39 0.0218(9) 0.0191(9) 0.0289(10) 0.0058(8) 0.0110(8) 0.0021(7)
C40 0.0238(10) 0.0200(10) 0.0318(11) 0.0071(8) 0.0082(8) 0.0020(8)
C41 0.0282(11) 0.0313(12) 0.0268(11) 0.0109(9) 0.0048(9) -0.0002(9)
C42 0.0373(14) 0.0485(16) 0.0454(16) 0.0238(13) -0.0081(12) -0.0104(12)
C43 0.0354(13) 0.0444(15) 0.0392(14) 0.0138(12) 0.0035(11) 0.0135(11)
C44 0.0488(15) 0.0430(15) 0.0317(13) 0.0149(11) 0.0107(11) 0.0054(12)
O1A 0.054(3) 0.090(4) 0.049(3) 0.014(3) 0.027(2) -0.007(3)
C1A 0.039(4) 0.046(6) 0.037(4) 0.022(4) 0.008(3) -0.006(4)
C2A 0.067(4) 0.047(3) 0.027(3) 0.011(2) 0.008(3) -0.002(3)
C3A 0.057(8) 0.083(8) 0.059(8) -0.014(6) -0.019(5) 0.017(6)
C4A 0.053(5) 0.189(12) 0.057(5) 0.004(6) 0.016(4) -0.058(6)
C5A 0.044(4) 0.049(6) 0.040(4) 0.020(4) 0.017(3) 0.011(4)
C6A 0.047(4) 0.184(11) 0.031(3) 0.004(5) 0.002(3) -0.038(5)
C7A 0.035(5) 0.120(11) 0.033(5) 0.037(6) 0.006(4) -0.037(5)
C8A 0.045(4) 0.034(4) 0.221(14) -0.018(6) 0.023(6) -0.003(3)
C9A 0.048(4) 0.152(11) 0.219(15) 0.153(11) -0.016(6) -0.013(5)
C10A 0.050(4) 0.049(4) 0.059(4) 0.015(3) -0.014(3) 0.000(3)

_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.390(3) . ?
O2 C23 1.385(3) . ?
O3 C12 1.385(3) . ?
O4 C34 1.379(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.400(3) . ?
C2 C3 1.395(3) . ?
C2 C40 1.523(3) . ?
C3 C4 1.393(3) . ?
C4 C5 1.402(3) . ?
C4 C8 1.536(3) . ?
C5 C6 1.391(3) . ?
C6 C7 1.524(3) . ?
C7 C13 1.527(3) . ?
C8 C9 1.520(4) . ?
C8 C10 1.537(4) . ?
C8 C11 1.537(4) . ?
C12 C17 1.396(3) . ?
C12 C13 1.404(3) . ?
C13 C14 1.382(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.396(3) . ?
C15 C19 1.527(4) . ?
C15 C19B 1.57(4) . ?
C16 C17 1.392(3) . ?
C17 C18 1.522(3) . ?
C18 C24 1.525(3) . ?
C19 C22 1.527(4) . ?
C19 C20 1.531(4) . ?
C19 C21 1.533(4) . ?
C19B C22B 1.524(16) . ?
C19B C21B 1.525(16) . ?
C19B C20B 1.527(16) . ?
C23 C28 1.398(3) . ?
C23 C24 1.400(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.403(3) . ?
C26 C27 1.398(3) . ?
C26 C30 1.533(3) . ?
C27 C28 1.399(3) . ?
C28 C29 1.524(3) . ?
C29 C35 1.524(3) . ?
C30 C31 1.526(4) . ?
C30 C33 1.531(4) . ?
C30 C32 1.546(4) . ?
C34 C35 1.400(3) . ?
C34 C39 1.402(3) . ?
C35 C36 1.402(3) . ?
C36 C37 1.395(3) . ?
C37 C38 1.399(3) . ?
C37 C41 1.540(3) . ?
C38 C39 1.389(3) . ?
C39 C40 1.522(3) . ?
C41 C44 1.531(4) . ?
C41 C42 1.532(3) . ?
C41 C43 1.538(4) . ?
O1A C1A 1.388(12) . ?
C1A C6A 1.452(13) . ?
C1A C2A 1.498(11) . ?
C2A C3A 1.419(12) . ?
C3A C4A 1.455(13) . ?
C3A C10A 1.482(11) . ?
C4A C5A 1.497(13) . ?
C5A C6A 1.497(12) . ?
C6A C7A 1.520(10) . ?
C7A C8A 1.485(13) . ?
C7A C9A 1.521(12) . ?

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
O1 C1 C2 118.21(19) . . ?
O1 C1 C6 120.08(19) . . ?
C2 C1 C6 121.7(2) . . ?
C1 C2 C3 118.18(19) . . ?
C1 C2 C40 122.0(2) . . ?
C3 C2 C40 119.84(19) . . ?
C4 C3 C2 122.4(2) . . ?
C3 C4 C5 117.2(2) . . ?
C3 C4 C8 123.1(2) . . ?
C5 C4 C8 119.7(2) . . ?
C6 C5 C4 122.6(2) . . ?
C5 C6 C1 117.86(19) . . ?
C5 C6 C7 120.18(19) . . ?
C1 C6 C7 121.95(19) . . ?
C6 C7 C13 112.79(17) . . ?
C9 C8 C4 112.4(2) . . ?
C9 C8 C10 108.6(3) . . ?
C4 C8 C10 108.9(2) . . ?
C9 C8 C11 107.8(3) . . ?
C4 C8 C11 110.6(2) . . ?
C10 C8 C11 108.5(2) . . ?
O3 C12 C17 120.33(19) . . ?
O3 C12 C13 118.41(19) . . ?
C17 C12 C13 121.2(2) . . ?
C14 C13 C12 118.01(19) . . ?
C14 C13 C7 120.47(19) . . ?
C12 C13 C7 121.51(19) . . ?
C13 C14 C15 123.1(2) . . ?
C16 C15 C14 116.7(2) . . ?
C16 C15 C19 123.2(2) . . ?
C14 C15 C19 120.1(2) . . ?
C16 C15 C19B 115.3(9) . . ?
C14 C15 C19B 128.0(9) . . ?
C19 C15 C19B 8.1(9) . . ?
C17 C16 C15 122.7(2) . . ?
C16 C17 C12 118.20(19) . . ?
C16 C17 C18 119.6(2) . . ?
C12 C17 C18 122.2(2) . . ?
C17 C18 C24 112.77(17) . . ?
C22 C19 C15 112.1(2) . . ?
C22 C19 C20 108.6(3) . . ?
C15 C19 C20 109.5(2) . . ?
C22 C19 C21 108.9(3) . . ?
C15 C19 C21 109.3(2) . . ?
C20 C19 C21 108.4(3) . . ?
C22B C19B C21B 109.6(17) . . ?
C22B C19B C20B 108.8(17) . . ?
C21B C19B C20B 108.8(17) . . ?
C22B C19B C15 109.9(16) . . ?
C21B C19B C15 109.8(16) . . ?
C20B C19B C15 109.9(16) . . ?
O2 C23 C28 120.41(19) . . ?
O2 C23 C24 117.94(19) . . ?
C28 C23 C24 121.6(2) . . ?
C25 C24 C23 118.32(19) . . ?
C25 C24 C18 120.40(19) . . ?
C23 C24 C18 121.3(2) . . ?
C24 C25 C26 122.7(2) . . ?
C27 C26 C25 116.8(2) . . ?
C27 C26 C30 123.74(19) . . ?
C25 C26 C30 119.40(19) . . ?
C26 C27 C28 122.8(2) . . ?
C23 C28 C27 117.63(19) . . ?
C23 C28 C29 122.36(19) . . ?
C27 C28 C29 119.98(18) . . ?
C35 C29 C28 115.53(16) . . ?
C31 C30 C33 109.0(2) . . ?
C31 C30 C26 112.2(2) . . ?
C33 C30 C26 109.9(2) . . ?
C31 C30 C32 108.1(2) . . ?
C33 C30 C32 108.7(2) . . ?
C26 C30 C32 108.9(2) . . ?
O4 C34 C35 118.22(19) . . ?
O4 C34 C39 119.99(19) . . ?
C35 C34 C39 121.74(19) . . ?
C34 C35 C36 117.36(19) . . ?
C34 C35 C29 122.28(19) . . ?
C36 C35 C29 120.36(18) . . ?
C37 C36 C35 122.93(19) . . ?
C36 C37 C38 117.1(2) . . ?
C36 C37 C41 123.73(19) . . ?
C38 C37 C41 119.2(2) . . ?
C39 C38 C37 122.6(2) . . ?
C38 C39 C34 118.17(19) . . ?
C38 C39 C40 120.10(19) . . ?
C34 C39 C40 121.7(2) . . ?
C39 C40 C2 113.45(17) . . ?
C44 C41 C42 108.5(2) . . ?
C44 C41 C43 108.6(2) . . ?
C42 C41 C43 108.0(2) . . ?
C44 C41 C37 110.3(2) . . ?
C42 C41 C37 112.3(2) . . ?
C43 C41 C37 109.02(19) . . ?
O1A C1A C6A 118.5(8) . . ?
O1A C1A C2A 112.3(9) . . ?
C6A C1A C2A 116.3(8) . . ?
C3A C2A C1A 118.0(7) . . ?
C2A C3A C4A 118.2(8) . . ?
C2A C3A C10A 119.9(8) . . ?
C4A C3A C10A 116.8(9) . . ?
C3A C4A C5A 116.2(9) . . ?
C6A C5A C4A 115.1(9) . . ?
C1A C6A C5A 112.4(8) . . ?
C1A C6A C7A 114.7(7) . . ?
C5A C6A C7A 119.3(8) . . ?
C8A C7A C6A 114.7(9) . . ?
C8A C7A C9A 108.5(10) . . ?
C6A C7A C9A 108.4(9) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 28.75
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 0.438
_refine_diff_density_min -0.489
_refine_diff_density_rms 0.060


data_ku99
_database_code_depnum_ccdc_archive 'CCDC 603038'

_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common 't-bu-calix[4]arene azobenzene'
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C50 H61 N O4'
_chemical_formula_weight 740.00

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'

_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a 12.7011(19)
_cell_length_b 27.117(4)
_cell_length_c 12.7935(19)
_cell_angle_alpha 90.00
_cell_angle_beta 90.649(4)
_cell_angle_gamma 90.00
_cell_volume 4406.0(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?

_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.116
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1600
_exptl_absorpt_coefficient_mu 0.069
_exptl_absorpt_correction_type multiscan
_exptl_absorpt_correction_T_min 0.9695
_exptl_absorpt_correction_T_max 0.9863
_exptl_absorpt_process_details sadabs

_exptl_special_details
;
?
;

_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 31395
_diffrn_reflns_av_R_equivalents 0.2015
_diffrn_reflns_av_sigmaI/netI 0.1642
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.50
_diffrn_reflns_theta_max 22.50
_reflns_number_total 5755
_reflns_number_gt 2366
_reflns_threshold_expression >2sigma(I)

_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?

_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5755
_refine_ls_number_parameters 544
_refine_ls_number_restraints 90
_refine_ls_R_factor_all 0.1877
_refine_ls_R_factor_gt 0.0675
_refine_ls_wR_factor_ref 0.1269
_refine_ls_wR_factor_gt 0.1023
_refine_ls_goodness_of_fit_ref 0.851
_refine_ls_restrained_S_all 0.857
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.9558(2) 0.22318(11) 0.3791(2) 0.0387(9) Uani 1 1 d . . .
H1 H 1.0161 0.2228 0.4070 0.046 Uiso 1 1 calc R . .
O2 O 1.0228(2) 0.22703(11) 0.1797(2) 0.0382(9) Uani 1 1 d . . .
H2 H 0.9894 0.2225 0.2352 0.046 Uiso 1 1 calc R . .
O3 O 1.2210(2) 0.23069(11) 0.2495(2) 0.0376(8) Uani 1 1 d . . .
H3 H 1.1645 0.2274 0.2155 0.045 Uiso 1 1 calc R . .
O4 O 1.1551(2) 0.22639(11) 0.4481(2) 0.0401(9) Uani 1 1 d . . .
H4 H 1.1818 0.2266 0.3883 0.048 Uiso 1 1 calc R . .
C1 C 0.9017(3) 0.26502(17) 0.4119(4) 0.0310(12) Uani 1 1 d . . .
C2 C 0.9194(3) 0.28475(16) 0.5104(4) 0.0287(12) Uani 1 1 d . . .
C3 C 0.8573(3) 0.32541(16) 0.5402(4) 0.0327(13) Uani 1 1 d . . .
H3A H 0.8663 0.3385 0.6086 0.039 Uiso 1 1 calc R . .
C4 C 0.7840(3) 0.34695(16) 0.4739(4) 0.0318(12) Uani 1 1 d . . .
C5 C 0.7732(3) 0.32578(17) 0.3743(4) 0.0342(13) Uani 1 1 d . . .
H5 H 0.7235 0.3398 0.3268 0.041 Uiso 1 1 calc R . .
C6 C 0.8310(3) 0.28587(17) 0.3417(4) 0.0306(12) Uani 1 1 d . . .
C7 C 0.8151(3) 0.26620(16) 0.2308(3) 0.0333(13) Uani 1 1 d . . .
H7A H 0.8260 0.2300 0.2306 0.040 Uiso 1 1 calc R . .
H7B H 0.7418 0.2728 0.2076 0.040 Uiso 1 1 calc R . .
C8 C 0.7159(3) 0.39064(17) 0.5047(4) 0.0369(13) Uani 1 1 d . . .
C9 C 0.7355(4) 0.43386(17) 0.4308(4) 0.0602(16) Uani 1 1 d . . .
H9A H 0.6903 0.4616 0.4501 0.072 Uiso 1 1 calc R . .
H9B H 0.7193 0.4238 0.3588 0.072 Uiso 1 1 calc R . .
H9C H 0.8095 0.4439 0.4360 0.072 Uiso 1 1 calc R . .
C10 C 0.7386(4) 0.40819(18) 0.6160(4) 0.0655(18) Uani 1 1 d . . .
H10A H 0.7244 0.3814 0.6652 0.079 Uiso 1 1 calc R . .
H10B H 0.6935 0.4364 0.6320 0.079 Uiso 1 1 calc R . .
H10C H 0.8127 0.4180 0.6223 0.079 Uiso 1 1 calc R . .
C11 C 0.5999(3) 0.37627(17) 0.4978(4) 0.0524(15) Uani 1 1 d . . .
H11A H 0.5857 0.3500 0.5483 0.063 Uiso 1 1 calc R . .
H11B H 0.5834 0.3645 0.4270 0.063 Uiso 1 1 calc R . .
H11C H 0.5562 0.4051 0.5136 0.063 Uiso 1 1 calc R . .
C12 C 0.9897(4) 0.27079(17) 0.1333(3) 0.0318(12) Uani 1 1 d . . .
C13 C 0.8909(3) 0.29009(16) 0.1546(3) 0.0265(12) Uani 1 1 d . . .
C14 C 0.8618(3) 0.33288(17) 0.1030(4) 0.0369(13) Uani 1 1 d . . .
H14 H 0.7933 0.3458 0.1143 0.044 Uiso 1 1 calc R . .
C15 C 0.9285(4) 0.35809(17) 0.0350(4) 0.0357(13) Uani 1 1 d . . .
C16 C 1.0263(3) 0.33671(17) 0.0176(3) 0.0331(13) Uani 1 1 d . . .
H16 H 1.0728 0.3526 -0.0293 0.040 Uiso 1 1 calc R . .
C17 C 1.0594(3) 0.29360(17) 0.0651(3) 0.0287(12) Uani 1 1 d . . .
C18 C 1.1699(3) 0.27399(16) 0.0474(3) 0.0350(13) Uani 1 1 d . . .
H18A H 1.1693 0.2377 0.0548 0.042 Uiso 1 1 calc R . .
H18B H 1.1911 0.2818 -0.0250 0.042 Uiso 1 1 calc R . .
C19 C 0.8908(4) 0.40541(19) -0.0188(4) 0.0501(15) Uani 1 1 d . . .
C20 C 0.9787(4) 0.43205(19) -0.0719(5) 0.088(2) Uani 1 1 d . . .
H20A H 1.0046 0.4120 -0.1299 0.106 Uiso 1 1 calc R . .
H20B H 1.0361 0.4379 -0.0217 0.106 Uiso 1 1 calc R . .
H20C H 0.9529 0.4637 -0.0990 0.106 Uiso 1 1 calc R . .
C21 C 0.8495(4) 0.44157(19) 0.0657(5) 0.079(2) Uani 1 1 d . . .
H21A H 0.8297 0.4729 0.0326 0.095 Uiso 1 1 calc R . .
H21B H 0.9049 0.4475 0.1181 0.095 Uiso 1 1 calc R . .
H21C H 0.7879 0.4272 0.0995 0.095 Uiso 1 1 calc R . .
C22 C 0.8005(4) 0.3946(2) -0.0913(4) 0.092(2) Uani 1 1 d . . .
H22A H 0.7696 0.4256 -0.1161 0.111 Uiso 1 1 calc R . .
H22B H 0.7470 0.3755 -0.0543 0.111 Uiso 1 1 calc R . .
H22C H 0.8256 0.3755 -0.1511 0.111 Uiso 1 1 calc R . .
C23 C 1.2696(3) 0.27478(16) 0.2214(4) 0.0296(12) Uani 1 1 d . A .
C24 C 1.2506(3) 0.29549(17) 0.1232(4) 0.0326(12) Uani 1 1 d . . .
C25 C 1.3058(3) 0.33775(17) 0.0986(4) 0.0359(13) Uani 1 1 d . A .
H25 H 1.2948 0.3520 0.0315 0.043 Uiso 1 1 calc R . .
C26 C 1.3770(3) 0.36069(17) 0.1669(4) 0.0368(13) Uani 1 1 d D . .
C27 C 1.3900(3) 0.33836(18) 0.2646(4) 0.0385(13) Uani 1 1 d . A .
H27 H 1.4373 0.3532 0.3132 0.046 Uiso 1 1 calc R . .
C28 C 1.3380(3) 0.29586(18) 0.2947(4) 0.0349(13) Uani 1 1 d . . .
C29 C 1.3555(3) 0.27360(17) 0.4030(3) 0.0376(13) Uani 1 1 d . A .
H29A H 1.4280 0.2813 0.4272 0.045 Uiso 1 1 calc R . .
H29B H 1.3491 0.2373 0.3981 0.045 Uiso 1 1 calc R . .
C34 C 1.1810(4) 0.26958(17) 0.4996(4) 0.0322(12) Uani 1 1 d . A .
C35 C 1.2772(3) 0.29274(17) 0.4837(3) 0.0314(12) Uani 1 1 d . . .
C36 C 1.2997(3) 0.33458(17) 0.5417(4) 0.0352(13) Uani 1 1 d . A .
H36 H 1.3647 0.3509 0.5299 0.042 Uiso 1 1 calc R . .
C37 C 1.2328(3) 0.35422(17) 0.6163(3) 0.0345(13) Uani 1 1 d D . .
C38 C 1.1370(3) 0.32937(16) 0.6276(3) 0.0319(12) Uani 1 1 d . A .
H38 H 1.0883 0.3417 0.6770 0.038 Uiso 1 1 calc R . .
C39 C 1.1093(3) 0.28804(16) 0.5709(4) 0.0291(12) Uani 1 1 d . . .
C40 C 1.0013(3) 0.26407(16) 0.5862(3) 0.0356(13) Uani 1 1 d . A .
H40A H 1.0074 0.2280 0.5755 0.043 Uiso 1 1 calc R . .
H40B H 0.9781 0.2698 0.6588 0.043 Uiso 1 1 calc R . .
C30 C 1.4394(8) 0.4073(4) 0.1434(7) 0.0470(18) Uani 0.68 1 d PD A -1
C31 C 1.4014(8) 0.4302(3) 0.0402(6) 0.086(5) Uani 0.68 1 d PD A -1
H31A H 1.4170 0.4077 -0.0176 0.103 Uiso 0.68 1 calc PR A -1
H31B H 1.4375 0.4616 0.0292 0.103 Uiso 0.68 1 calc PR A -1
H31C H 1.3252 0.4358 0.0429 0.103 Uiso 0.68 1 calc PR A -1
C32 C 1.5553(5) 0.3928(3) 0.1370(7) 0.075(3) Uani 0.68 1 d PD A -1
H32A H 1.5813 0.3834 0.2066 0.090 Uiso 0.68 1 calc PR A -1
H32B H 1.5961 0.4208 0.1111 0.090 Uiso 0.68 1 calc PR A -1
H32C H 1.5628 0.3648 0.0891 0.090 Uiso 0.68 1 calc PR A -1
C33 C 1.4263(6) 0.4459(3) 0.2299(6) 0.070(3) Uani 0.68 1 d PD A -1
H33A H 1.3519 0.4552 0.2347 0.084 Uiso 0.68 1 calc PR A -1
H33B H 1.4683 0.4751 0.2134 0.084 Uiso 0.68 1 calc PR A -1
H33C H 1.4502 0.4320 0.2968 0.084 Uiso 0.68 1 calc PR A -1
C30A C 1.4428(15) 0.4046(9) 0.1238(14) 0.0470(18) Uani 0.32 1 d PD A -2
C31A C 1.3691(15) 0.4467(6) 0.0910(15) 0.086(5) Uani 0.32 1 d PD A -2
H31D H 1.3318 0.4589 0.1524 0.103 Uiso 0.32 1 calc PR A -2
H31E H 1.3179 0.4345 0.0392 0.103 Uiso 0.32 1 calc PR A -2
H31F H 1.4103 0.4735 0.0604 0.103 Uiso 0.32 1 calc PR A -2
C32A C 1.5089(11) 0.3894(6) 0.0301(11) 0.075(3) Uani 0.32 1 d PD A -2
H32D H 1.5521 0.4173 0.0078 0.090 Uiso 0.32 1 calc PR A -2
H32E H 1.4623 0.3793 -0.0276 0.090 Uiso 0.32 1 calc PR A -2
H32F H 1.5547 0.3618 0.0499 0.090 Uiso 0.32 1 calc PR A -2
C33A C 1.5175(13) 0.4240(6) 0.2091(12) 0.070(3) Uani 0.32 1 d PD A -2
H33D H 1.5651 0.4485 0.1791 0.084 Uiso 0.32 1 calc PR A -2
H33E H 1.5588 0.3965 0.2380 0.084 Uiso 0.32 1 calc PR A -2
H33F H 1.4765 0.4393 0.2649 0.084 Uiso 0.32 1 calc PR A -2
C41 C 1.2578(5) 0.3984(3) 0.6854(6) 0.0393(15) Uani 0.76 1 d PD A -3
C42 C 1.3666(5) 0.4204(2) 0.6644(6) 0.065(2) Uani 0.76 1 d PD A -3
H42A H 1.4208 0.3953 0.6769 0.078 Uiso 0.76 1 calc PR A -3
H42B H 1.3788 0.4485 0.7112 0.078 Uiso 0.76 1 calc PR A -3
H42C H 1.3698 0.4316 0.5916 0.078 Uiso 0.76 1 calc PR A -3
C43 C 1.2563(5) 0.3829(2) 0.8018(4) 0.0498(18) Uani 0.76 1 d PD A -3
H43A H 1.1860 0.3708 0.8194 0.060 Uiso 0.76 1 calc PR A -3
H43B H 1.2738 0.4114 0.8458 0.060 Uiso 0.76 1 calc PR A -3
H43C H 1.3082 0.3567 0.8139 0.060 Uiso 0.76 1 calc PR A -3
C44 C 1.1755(4) 0.4392(2) 0.6710(5) 0.054(2) Uani 0.76 1 d PD A -3
H44A H 1.1747 0.4502 0.5980 0.064 Uiso 0.76 1 calc PR A -3
H44B H 1.1934 0.4671 0.7166 0.064 Uiso 0.76 1 calc PR A -3
H44C H 1.1059 0.4265 0.6893 0.064 Uiso 0.76 1 calc PR A -3
C41A C 1.2738(15) 0.3985(10) 0.6757(17) 0.0393(15) Uani 0.24 1 d PD A -4
C42A C 1.3002(15) 0.4396(5) 0.5977(13) 0.065(2) Uani 0.24 1 d PD A -4
H42D H 1.3552 0.4281 0.5504 0.078 Uiso 0.24 1 calc PR A -4
H42E H 1.3254 0.4687 0.6359 0.078 Uiso 0.24 1 calc PR A -4
H42F H 1.2370 0.4482 0.5572 0.078 Uiso 0.24 1 calc PR A -4
C43A C 1.3715(11) 0.3841(6) 0.7410(13) 0.0498(18) Uani 0.24 1 d PD A -4
H43D H 1.3569 0.3538 0.7800 0.060 Uiso 0.24 1 calc PR A -4
H43E H 1.3887 0.4107 0.7902 0.060 Uiso 0.24 1 calc PR A -4
H43F H 1.4312 0.3786 0.6946 0.060 Uiso 0.24 1 calc PR A -4
C44A C 1.1873(13) 0.4169(7) 0.7491(13) 0.054(2) Uani 0.24 1 d PD A -4
H44D H 1.1334 0.4345 0.7084 0.064 Uiso 0.24 1 calc PR A -4
H44E H 1.2183 0.4392 0.8013 0.064 Uiso 0.24 1 calc PR A -4
H44F H 1.1552 0.3887 0.7845 0.064 Uiso 0.24 1 calc PR A -4
N1G N 1.0198(3) 0.50638(18) 0.4609(3) 0.0583(13) Uani 1 1 d . B -5
C1G C 1.0473(3) 0.46297(19) 0.3956(4) 0.0387(14) Uani 1 1 d . B -5
C2G C 1.0876(4) 0.47621(19) 0.2999(4) 0.0525(15) Uani 1 1 d . B -5
H2G H 1.0948 0.5100 0.2820 0.063 Uiso 1 1 calc R B -5
C3G C 1.1174(4) 0.4400(3) 0.2306(4) 0.0649(17) Uani 1 1 d . B -5
H3G H 1.1450 0.4488 0.1644 0.078 Uiso 1 1 calc R B -5
C4G C 1.1071(4) 0.3917(2) 0.2573(5) 0.0581(17) Uani 1 1 d . B -5
H4G H 1.1283 0.3667 0.2101 0.070 Uiso 1 1 calc R B -5
C5G C 1.0668(4) 0.3793(2) 0.3508(5) 0.0524(16) Uani 1 1 d . B -5
H5G H 1.0594 0.3454 0.3683 0.063 Uiso 1 1 calc R B -5
C6G C 1.0364(4) 0.4145(2) 0.4207(4) 0.0486(15) Uani 1 1 d . B -5
H6G H 1.0080 0.4052 0.4862 0.058 Uiso 1 1 calc R B -5

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.032(2) 0.039(2) 0.045(2) -0.0009(18) -0.0007(17) 0.0001(17)
O2 0.039(2) 0.039(2) 0.036(2) 0.0013(18) 0.0044(17) -0.0027(17)
O3 0.033(2) 0.045(2) 0.034(2) -0.0020(18) 0.0015(16) 0.0025(17)
O4 0.043(2) 0.046(2) 0.032(2) -0.0023(19) 0.0020(18) 0.0024(17)
C1 0.020(3) 0.034(3) 0.038(4) 0.008(3) 0.007(3) 0.001(2)
C2 0.026(3) 0.035(3) 0.025(3) 0.007(3) 0.001(2) -0.009(2)
C3 0.032(3) 0.039(3) 0.027(3) -0.004(3) 0.010(3) -0.008(3)
C4 0.027(3) 0.036(3) 0.032(3) 0.004(3) 0.001(3) -0.009(2)
C5 0.021(3) 0.049(4) 0.032(4) 0.010(3) -0.008(3) -0.009(3)
C6 0.024(3) 0.033(3) 0.035(3) 0.007(3) 0.004(3) -0.004(2)
C7 0.028(3) 0.037(3) 0.036(4) -0.002(3) 0.001(3) -0.006(2)
C8 0.034(3) 0.037(3) 0.040(4) -0.001(3) 0.002(3) 0.001(3)
C9 0.054(4) 0.056(4) 0.071(5) 0.005(3) 0.002(3) 0.007(3)
C10 0.061(4) 0.065(4) 0.070(5) -0.023(4) -0.015(3) 0.021(3)
C11 0.041(3) 0.063(4) 0.053(4) 0.001(3) 0.005(3) 0.007(3)
C12 0.040(3) 0.030(3) 0.025(3) -0.003(3) -0.008(3) 0.008(3)
C13 0.029(3) 0.031(3) 0.019(3) -0.001(2) -0.007(2) -0.004(2)
C14 0.027(3) 0.051(4) 0.033(3) 0.000(3) -0.011(3) 0.004(3)
C15 0.031(3) 0.045(3) 0.031(3) 0.008(3) -0.002(3) -0.001(3)
C16 0.027(3) 0.047(3) 0.025(3) 0.009(3) 0.006(2) -0.006(3)
C17 0.033(3) 0.036(3) 0.017(3) -0.002(3) 0.009(2) -0.005(3)
C18 0.045(3) 0.037(3) 0.023(3) -0.009(3) 0.005(3) 0.002(3)
C19 0.040(4) 0.056(4) 0.054(4) 0.020(3) 0.005(3) 0.005(3)
C20 0.065(4) 0.073(5) 0.127(6) 0.055(4) 0.029(4) 0.022(3)
C21 0.062(4) 0.068(4) 0.107(6) 0.022(4) 0.009(4) 0.014(3)
C22 0.095(5) 0.096(5) 0.085(5) 0.044(4) -0.035(4) 0.003(4)
C23 0.023(3) 0.026(3) 0.040(4) 0.000(3) 0.012(3) -0.003(2)
C24 0.029(3) 0.038(3) 0.031(3) 0.000(3) 0.003(3) 0.012(3)
C25 0.029(3) 0.045(3) 0.034(3) 0.004(3) 0.009(3) 0.009(3)
C26 0.028(3) 0.045(3) 0.037(4) -0.001(3) -0.005(3) 0.000(3)
C27 0.027(3) 0.053(4) 0.035(4) -0.010(3) -0.008(3) 0.002(3)
C28 0.026(3) 0.041(3) 0.038(4) -0.001(3) 0.000(3) 0.007(3)
C29 0.025(3) 0.057(3) 0.031(3) 0.001(3) 0.002(2) 0.004(3)
C34 0.036(3) 0.036(3) 0.024(3) -0.002(3) -0.006(3) 0.008(3)
C35 0.030(3) 0.042(3) 0.023(3) 0.003(3) 0.007(2) 0.003(3)
C36 0.032(3) 0.044(3) 0.029(3) 0.010(3) 0.001(3) 0.003(3)
C37 0.030(3) 0.044(3) 0.029(3) -0.002(3) 0.001(3) -0.002(3)
C38 0.026(3) 0.047(3) 0.023(3) 0.005(3) 0.005(2) 0.006(3)
C39 0.032(3) 0.033(3) 0.022(3) 0.004(3) 0.001(3) 0.002(3)
C40 0.037(3) 0.045(3) 0.025(3) 0.008(3) -0.002(3) 0.001(3)
C30 0.039(4) 0.058(4) 0.043(5) 0.004(4) -0.009(3) -0.015(3)
C31 0.094(8) 0.092(8) 0.070(10) 0.041(7) -0.015(7) -0.054(6)
C32 0.036(5) 0.094(7) 0.096(8) 0.004(7) 0.021(5) -0.028(5)
C33 0.087(7) 0.054(6) 0.069(6) 0.008(5) -0.015(6) -0.018(5)
C30A 0.039(4) 0.058(4) 0.043(5) 0.004(4) -0.009(3) -0.015(3)
C31A 0.094(8) 0.092(8) 0.070(10) 0.041(7) -0.015(7) -0.054(6)
C32A 0.036(5) 0.094(7) 0.096(8) 0.004(7) 0.021(5) -0.028(5)
C33A 0.087(7) 0.054(6) 0.069(6) 0.008(5) -0.015(6) -0.018(5)
C41 0.021(4) 0.045(3) 0.052(4) -0.001(3) -0.002(3) -0.005(3)
C42 0.051(5) 0.072(6) 0.073(7) -0.035(5) 0.008(4) -0.012(4)
C43 0.059(5) 0.055(5) 0.035(5) -0.011(4) 0.003(4) 0.002(4)
C44 0.053(5) 0.052(5) 0.055(6) -0.016(4) -0.005(4) 0.004(4)
C41A 0.021(4) 0.045(3) 0.052(4) -0.001(3) -0.002(3) -0.005(3)
C42A 0.051(5) 0.072(6) 0.073(7) -0.035(5) 0.008(4) -0.012(4)
C43A 0.059(5) 0.055(5) 0.035(5) -0.011(4) 0.003(4) 0.002(4)
C44A 0.053(5) 0.052(5) 0.055(6) -0.016(4) -0.005(4) 0.004(4)
N1G 0.055(3) 0.077(4) 0.043(4) 0.019(3) -0.004(3) -0.004(3)
C1G 0.038(3) 0.042(4) 0.036(4) -0.022(3) -0.001(3) 0.010(3)
C2G 0.067(4) 0.047(4) 0.043(4) 0.007(3) 0.007(3) 0.005(3)
C3G 0.066(4) 0.092(5) 0.037(4) 0.001(4) 0.022(3) 0.007(4)
C4G 0.066(4) 0.064(5) 0.044(5) -0.027(4) -0.005(3) 0.021(4)
C5G 0.054(4) 0.045(4) 0.059(5) -0.011(4) -0.003(3) 0.000(3)
C6G 0.047(4) 0.049(4) 0.049(4) 0.008(3) 0.005(3) 0.002(3)

_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.394(5) . ?
O2 C12 1.390(5) . ?
O3 C23 1.394(5) . ?
O4 C34 1.381(5) . ?
C1 C6 1.382(6) . ?
C1 C2 1.385(6) . ?
C2 C3 1.410(5) . ?
C2 C40 1.522(5) . ?
C3 C4 1.382(5) . ?
C4 C5 1.404(6) . ?
C4 C8 1.521(6) . ?
C5 C6 1.375(6) . ?
C6 C7 1.528(6) . ?
C7 C13 1.523(5) . ?
C8 C11 1.525(5) . ?
C8 C10 1.526(6) . ?
C8 C9 1.528(6) . ?
C12 C13 1.390(5) . ?
C12 C17 1.395(6) . ?
C13 C14 1.383(5) . ?
C14 C15 1.399(5) . ?
C15 C16 1.392(5) . ?
C15 C19 1.530(6) . ?
C16 C17 1.381(5) . ?
C17 C18 1.520(5) . ?
C18 C24 1.519(5) . ?
C19 C22 1.496(6) . ?
C19 C20 1.500(6) . ?
C19 C21 1.554(7) . ?
C23 C28 1.394(6) . ?
C23 C24 1.395(6) . ?
C24 C25 1.382(6) . ?
C25 C26 1.396(5) . ?
C26 C27 1.397(6) . ?
C26 C30 1.522(14) . ?
C26 C30A 1.56(3) . ?
C27 C28 1.385(6) . ?
C28 C29 1.525(6) . ?
C29 C35 1.532(5) . ?
C34 C39 1.389(6) . ?
C34 C35 1.391(6) . ?
C35 C36 1.384(6) . ?
C36 C37 1.390(5) . ?
C37 C38 1.400(5) . ?
C37 C41A 1.51(3) . ?
C37 C41 1.519(11) . ?
C38 C39 1.378(5) . ?
C39 C40 1.532(5) . ?
C30 C32 1.527(9) . ?
C30 C31 1.533(9) . ?
C30 C33 1.533(9) . ?
C30A C32A 1.529(15) . ?
C30A C33A 1.531(15) . ?
C30A C31A 1.531(15) . ?
C41 C42 1.533(8) . ?
C41 C44 1.533(8) . ?
C41 C43 1.548(8) . ?
C41A C42A 1.535(15) . ?
C41A C44A 1.537(15) . ?
C41A C43A 1.539(15) . ?
N1G C1G 1.487(6) . ?
C1G C6G 1.361(6) . ?
C1G C2G 1.380(6) . ?
C2G C3G 1.379(6) . ?
C3G C4G 1.361(7) . ?
C4G C5G 1.348(6) . ?
C5G C6G 1.366(6) . ?

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 C1 C2 122.0(4) . . ?
C6 C1 O1 117.2(4) . . ?
C2 C1 O1 120.8(4) . . ?
C1 C2 C3 117.6(4) . . ?
C1 C2 C40 122.7(4) . . ?
C3 C2 C40 119.7(4) . . ?
C4 C3 C2 122.6(4) . . ?
C3 C4 C5 116.3(4) . . ?
C3 C4 C8 123.5(4) . . ?
C5 C4 C8 120.2(4) . . ?
C6 C5 C4 123.4(4) . . ?
C5 C6 C1 118.1(5) . . ?
C5 C6 C7 119.4(4) . . ?
C1 C6 C7 122.6(4) . . ?
C13 C7 C6 111.6(3) . . ?
C4 C8 C11 109.8(4) . . ?
C4 C8 C10 112.4(4) . . ?
C11 C8 C10 107.8(4) . . ?
C4 C8 C9 109.9(4) . . ?
C11 C8 C9 108.9(4) . . ?
C10 C8 C9 107.9(4) . . ?
C13 C12 O2 120.5(4) . . ?
C13 C12 C17 122.4(4) . . ?
O2 C12 C17 117.1(4) . . ?
C14 C13 C12 117.4(4) . . ?
C14 C13 C7 119.7(4) . . ?
C12 C13 C7 123.0(4) . . ?
C13 C14 C15 123.1(4) . . ?
C16 C15 C14 116.3(4) . . ?
C16 C15 C19 123.6(4) . . ?
C14 C15 C19 120.0(4) . . ?
C17 C16 C15 123.4(4) . . ?
C16 C17 C12 117.3(4) . . ?
C16 C17 C18 120.5(4) . . ?
C12 C17 C18 122.1(4) . . ?
C24 C18 C17 112.8(3) . . ?
C22 C19 C20 112.5(5) . . ?
C22 C19 C15 110.4(4) . . ?
C20 C19 C15 112.1(4) . . ?
C22 C19 C21 107.0(4) . . ?
C20 C19 C21 105.7(5) . . ?
C15 C19 C21 108.9(4) . . ?
C28 C23 O3 116.8(4) . . ?
C28 C23 C24 122.8(4) . . ?
O3 C23 C24 120.4(4) . . ?
C25 C24 C23 117.1(4) . . ?
C25 C24 C18 120.9(4) . . ?
C23 C24 C18 121.9(4) . . ?
C24 C25 C26 123.6(5) . . ?
C25 C26 C27 115.8(4) . . ?
C25 C26 C30 125.5(5) . . ?
C27 C26 C30 118.7(5) . . ?
C25 C26 C30A 117.7(7) . . ?
C27 C26 C30A 126.1(7) . . ?
C30 C26 C30A 9.8(8) . . ?
C28 C27 C26 123.9(4) . . ?
C27 C28 C23 116.7(5) . . ?
C27 C28 C29 121.1(4) . . ?
C23 C28 C29 122.2(4) . . ?
C28 C29 C35 112.9(4) . . ?
O4 C34 C39 117.7(4) . . ?
O4 C34 C35 121.1(4) . . ?
C39 C34 C35 121.1(4) . . ?
C36 C35 C34 117.9(4) . . ?
C36 C35 C29 120.5(4) . . ?
C34 C35 C29 121.6(4) . . ?
C35 C36 C37 123.9(4) . . ?
C36 C37 C38 115.1(4) . . ?
C36 C37 C41A 116.1(7) . . ?
C38 C37 C41A 128.7(7) . . ?
C36 C37 C41 125.1(5) . . ?
C38 C37 C41 119.7(5) . . ?
C41A C37 C41 9.1(8) . . ?
C39 C38 C37 123.6(4) . . ?
C38 C39 C34 118.2(4) . . ?
C38 C39 C40 120.1(4) . . ?
C34 C39 C40 121.7(4) . . ?
C2 C40 C39 111.7(4) . . ?
C26 C30 C32 107.6(7) . . ?
C26 C30 C31 110.3(7) . . ?
C32 C30 C31 110.6(8) . . ?
C26 C30 C33 111.3(7) . . ?
C32 C30 C33 109.1(7) . . ?
C31 C30 C33 108.0(8) . . ?
C32A C30A C33A 108.1(13) . . ?
C32A C30A C31A 109.0(14) . . ?
C33A C30A C31A 108.2(14) . . ?
C32A C30A C26 111.8(13) . . ?
C33A C30A C26 109.9(13) . . ?
C31A C30A C26 109.7(13) . . ?
C37 C41 C42 112.9(6) . . ?
C37 C41 C44 111.3(6) . . ?
C42 C41 C44 108.2(6) . . ?
C37 C41 C43 110.0(6) . . ?
C42 C41 C43 107.2(6) . . ?
C44 C41 C43 107.2(6) . . ?
C37 C41A C42A 109.1(14) . . ?
C37 C41A C44A 108.7(14) . . ?
C42A C41A C44A 109.0(15) . . ?
C37 C41A C43A 110.0(14) . . ?
C42A C41A C43A 110.9(15) . . ?
C44A C41A C43A 109.2(15) . . ?
C6G C1G C2G 120.0(5) . . ?
C6G C1G N1G 127.4(5) . . ?
C2G C1G N1G 112.6(5) . . ?
C3G C2G C1G 119.6(5) . . ?
C4G C3G C2G 119.7(5) . . ?
C5G C4G C3G 120.2(5) . . ?
C4G C5G C6G 121.3(6) . . ?
C1G C6G C5G 119.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 22.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.242
_refine_diff_density_min -0.190
_refine_diff_density_rms 0.041


data_ort
_database_code_depnum_ccdc_archive 'CCDC 603039'

_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common 't-bu-calix[4]arene mesitylene'
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C53 H68 O4'
_chemical_formula_weight 769.07

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'

_symmetry_cell_setting orhtorhombic
_symmetry_space_group_name_H-M 'P n a 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a 29.397(4)
_cell_length_b 12.4786(17)
_cell_length_c 12.7216(17)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 4666.7(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 4243
_cell_measurement_theta_min 1.6
_cell_measurement_theta_max 22.05

_exptl_crystal_description plate
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.095
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1672
_exptl_absorpt_coefficient_mu 0.067
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9834
_exptl_absorpt_correction_T_max 0.9960
_exptl_absorpt_process_details SADABS

_exptl_special_details
;
?
;

_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method '/w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 31808
_diffrn_reflns_av_R_equivalents 0.1453
_diffrn_reflns_av_sigmaI/netI 0.1025
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.60
_diffrn_reflns_theta_max 22.05
_reflns_number_total 6053
_reflns_number_gt 4096
_reflns_threshold_expression >2sigma(I)

_computing_data_collection SMART-CCD
_computing_cell_refinement 'SAINT (Bruker 2001)'
_computing_data_reduction 'SAINT (Bruker 2001)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?

_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+0.0796P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -3(3)
_refine_ls_number_reflns 6053
_refine_ls_number_parameters 547
_refine_ls_number_restraints 41
_refine_ls_R_factor_all 0.1133
_refine_ls_R_factor_gt 0.0704
_refine_ls_wR_factor_ref 0.1764
_refine_ls_wR_factor_gt 0.1593
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_restrained_S_all 1.063
_refine_ls_shift/su_max 0.023
_refine_ls_shift/su_mean 0.001

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 0.27171(11) 0.6754(3) 0.1914(3) 0.0288(10) Uani 1 1 d . . .
H1 H 0.2812 0.7157 0.2374 0.043 Uiso 1 1 calc R . .
O2 O 0.27413(12) 0.8810(3) 0.2571(3) 0.0322(10) Uani 1 1 d . . .
H2 H 0.2746 0.9095 0.1991 0.048 Uiso 1 1 calc R . .
O3 O 0.27143(11) 0.9463(3) 0.0576(3) 0.0312(10) Uani 1 1 d . . .
H3 H 0.2744 0.8919 0.0221 0.047 Uiso 1 1 calc R . .
O4 O 0.26888(12) 0.7414(3) -0.0081(3) 0.0311(10) Uani 1 1 d . . .
H4 H 0.2706 0.7153 0.0510 0.047 Uiso 1 1 calc R . .
C1 C 0.23114(17) 0.6279(4) 0.2246(4) 0.0223(14) Uani 1 1 d . A .
C2 C 0.20947(18) 0.5560(4) 0.1570(4) 0.0240(14) Uani 1 1 d . . .
C3 C 0.16947(18) 0.5094(4) 0.1926(5) 0.0292(15) Uani 1 1 d . A .
H3 H 0.1539 0.4630 0.1480 0.035 Uiso 1 1 calc R . .
C4 C 0.15158(16) 0.5289(4) 0.2918(4) 0.0287(15) Uani 1 1 d D . .
C5 C 0.17479(18) 0.5985(4) 0.3560(4) 0.0253(14) Uani 1 1 d . A .
H5 H 0.1631 0.6124 0.4226 0.030 Uiso 1 1 calc R . .
C6 C 0.21434(19) 0.6484(4) 0.3269(4) 0.0247(14) Uani 1 1 d . . .
C8 C 0.22676(19) 0.5355(4) 0.0469(4) 0.0289(15) Uani 1 1 d . A .
H8A H 0.2187 0.4632 0.0261 0.035 Uiso 1 1 calc R . .
H8B H 0.2597 0.5409 0.0465 0.035 Uiso 1 1 calc R . .
C7A C 0.10851(19) 0.4758(5) 0.3357(5) 0.0367(18) Uani 0.839(8) 1 d PD A 1
C9 C 0.0742(2) 0.5605(6) 0.3732(6) 0.054(3) Uani 0.839(8) 1 d PD A 1
H9A H 0.0475 0.5255 0.3998 0.080 Uiso 0.839(8) 1 calc PR A 1
H9B H 0.0660 0.6059 0.3154 0.080 Uiso 0.839(8) 1 calc PR A 1
H9C H 0.0878 0.6029 0.4279 0.080 Uiso 0.839(8) 1 calc PR A 1
C10 C 0.1217(2) 0.4016(5) 0.4277(5) 0.049(2) Uani 0.839(8) 1 d PD A 1
H10A H 0.0949 0.3672 0.4546 0.074 Uiso 0.839(8) 1 calc PR A 1
H10B H 0.1357 0.4431 0.4823 0.074 Uiso 0.839(8) 1 calc PR A 1
H10C H 0.1427 0.3482 0.4033 0.074 Uiso 0.839(8) 1 calc PR A 1
C11 C 0.0848(3) 0.4068(8) 0.2511(6) 0.084(4) Uani 0.839(8) 1 d PD A 1
H11A H 0.0582 0.3740 0.2807 0.126 Uiso 0.839(8) 1 calc PR A 1
H11B H 0.1053 0.3521 0.2272 0.126 Uiso 0.839(8) 1 calc PR A 1
H11C H 0.0762 0.4513 0.1929 0.126 Uiso 0.839(8) 1 calc PR A 1
C7B C 0.1094(4) 0.4598(10) 0.3106(12) 0.0367(18) Uani 0.161(8) 1 d PD A 2
C12 C 0.0947(13) 0.498(3) 0.4198(14) 0.10(2) Uiso 0.161(8) 1 d PD A 2
H12A H 0.0690 0.4568 0.4428 0.157 Uiso 0.161(8) 1 calc PR A 2
H12B H 0.0866 0.5723 0.4168 0.157 Uiso 0.161(8) 1 calc PR A 2
H12C H 0.1194 0.4882 0.4684 0.157 Uiso 0.161(8) 1 calc PR A 2
C13 C 0.1225(9) 0.3412(10) 0.310(3) 0.071(15) Uiso 0.161(8) 1 d PD A 2
H13A H 0.1335 0.3219 0.2415 0.106 Uiso 0.161(8) 1 calc PR A 2
H13B H 0.0964 0.2985 0.3269 0.106 Uiso 0.161(8) 1 calc PR A 2
H13C H 0.1459 0.3288 0.3611 0.106 Uiso 0.161(8) 1 calc PR A 2
C14 C 0.0722(7) 0.483(3) 0.2296(19) 0.10(2) Uiso 0.161(8) 1 d PD A 2
H14A H 0.0814 0.4556 0.1623 0.146 Uiso 0.161(8) 1 calc PR A 2
H14B H 0.0674 0.5587 0.2247 0.146 Uiso 0.161(8) 1 calc PR A 2
H14C H 0.0444 0.4485 0.2509 0.146 Uiso 0.161(8) 1 calc PR A 2
C21 C 0.23532(18) 0.9118(4) 0.3101(4) 0.0241(14) Uani 1 1 d . A .
C22 C 0.21686(18) 0.8426(4) 0.3836(4) 0.0256(15) Uani 1 1 d . . .
C23 C 0.17909(19) 0.8720(4) 0.4373(4) 0.0272(14) Uani 1 1 d . A .
H23 H 0.1668 0.8244 0.4858 0.033 Uiso 1 1 calc R . .
C24 C 0.15776(18) 0.9716(4) 0.4227(4) 0.0261(14) Uani 1 1 d . . .
C25 C 0.17689(18) 1.0395(4) 0.3486(4) 0.0204(13) Uani 1 1 d . A .
H25 H 0.1632 1.1055 0.3362 0.024 Uiso 1 1 calc R . .
C26 C 0.21534(18) 1.0129(4) 0.2927(4) 0.0236(14) Uani 1 1 d . . .
C27 C 0.11623(19) 0.9999(4) 0.4875(4) 0.0322(16) Uani 1 1 d . A .
C28 C 0.23704(19) 0.7301(4) 0.3988(4) 0.0249(15) Uani 1 1 d . A .
H28A H 0.2694 0.7321 0.3842 0.030 Uiso 1 1 calc R . .
H28B H 0.2331 0.7082 0.4714 0.030 Uiso 1 1 calc R . .
C29 C 0.0972(2) 1.1090(5) 0.4589(6) 0.061(2) Uani 1 1 d . . .
H29A H 0.0711 1.1239 0.5018 0.092 Uiso 1 1 calc R A .
H29B H 0.0884 1.1093 0.3862 0.092 Uiso 1 1 calc R . .
H29C H 0.1199 1.1628 0.4707 0.092 Uiso 1 1 calc R . .
C30 C 0.1291(2) 0.9997(5) 0.6037(5) 0.0481(18) Uani 1 1 d . . .
H30A H 0.1029 1.0180 0.6452 0.072 Uiso 1 1 calc R A .
H30B H 0.1528 1.0513 0.6158 0.072 Uiso 1 1 calc R . .
H30C H 0.1397 0.9297 0.6234 0.072 Uiso 1 1 calc R . .
C31 C 0.0788(2) 0.9143(6) 0.4705(5) 0.0501(19) Uani 1 1 d . . .
H31A H 0.0525 0.9325 0.5116 0.075 Uiso 1 1 calc R A .
H31B H 0.0900 0.8455 0.4920 0.075 Uiso 1 1 calc R . .
H31C H 0.0707 0.9120 0.3975 0.075 Uiso 1 1 calc R . .
C41 C 0.23154(18) 0.9991(5) 0.0284(5) 0.0275(15) Uani 1 1 d . A .
C42 C 0.21235(18) 1.0702(4) 0.1007(4) 0.0242(14) Uani 1 1 d . . .
C43 C 0.17316(18) 1.1258(4) 0.0700(4) 0.0247(15) Uani 1 1 d . A .
H43 H 0.1610 1.1762 0.1159 0.030 Uiso 1 1 calc R . .
C44 C 0.15190(18) 1.1093(4) -0.0249(4) 0.0243(14) Uani 1 1 d . . .
C45 C 0.17165(18) 1.0346(4) -0.0932(4) 0.0278(15) Uani 1 1 d . A .
H45 H 0.1578 1.0217 -0.1577 0.033 Uiso 1 1 calc R . .
C46 C 0.21093(19) 0.9793(4) -0.0683(4) 0.0257(14) Uani 1 1 d . . .
C47 C 0.1087(2) 1.1675(5) -0.0607(5) 0.0373(16) Uani 1 1 d . A .
C48 C 0.23334(17) 1.0884(4) 0.2076(4) 0.0209(13) Uani 1 1 d . A .
H48A H 0.2275 1.1618 0.2289 0.025 Uiso 1 1 calc R . .
H48B H 0.2660 1.0794 0.2021 0.025 Uiso 1 1 calc R . .
C49 C 0.0713(2) 1.0876(5) -0.0840(5) 0.0501(19) Uani 1 1 d . . .
H49A H 0.0642 1.0481 -0.0214 0.075 Uiso 1 1 calc R A .
H49B H 0.0813 1.0389 -0.1377 0.075 Uiso 1 1 calc R . .
H49C H 0.0447 1.1250 -0.1078 0.075 Uiso 1 1 calc R . .
C50 C 0.1190(2) 1.2307(5) -0.1611(5) 0.0444(18) Uani 1 1 d . . .
H50A H 0.1427 1.2818 -0.1473 0.067 Uiso 1 1 calc R A .
H50B H 0.0921 1.2675 -0.1837 0.067 Uiso 1 1 calc R . .
H50C H 0.1288 1.1822 -0.2152 0.067 Uiso 1 1 calc R . .
C51 C 0.0918(2) 1.2485(6) 0.0230(5) 0.055(2) Uani 1 1 d . . .
H51A H 0.1154 1.2995 0.0376 0.083 Uiso 1 1 calc R A .
H51B H 0.0841 1.2108 0.0864 0.083 Uiso 1 1 calc R . .
H51C H 0.0654 1.2852 -0.0031 0.083 Uiso 1 1 calc R . .
C61 C 0.22785(17) 0.7117(5) -0.0539(4) 0.0253(15) Uani 1 1 d . A .
C62 C 0.20826(19) 0.7864(4) -0.1241(4) 0.0208(14) Uani 1 1 d . . .
C63 C 0.1683(2) 0.7576(4) -0.1734(4) 0.0256(14) Uani 1 1 d . A .
H63 H 0.1557 0.8047 -0.2220 0.031 Uiso 1 1 calc R . .
C64 C 0.14589(16) 0.6620(4) -0.1541(4) 0.0314(15) Uani 1 1 d D . .
C65 C 0.16660(19) 0.5918(4) -0.0839(4) 0.0304(16) Uani 1 1 d . A .
H65 H 0.1525 0.5264 -0.0705 0.036 Uiso 1 1 calc R . .
C66 C 0.20722(19) 0.6144(4) -0.0329(4) 0.0250(14) Uani 1 1 d . . .
C68 C 0.22937(18) 0.8952(4) -0.1448(4) 0.0264(15) Uani 1 1 d . A .
H68A H 0.2227 0.9171 -0.2164 0.032 Uiso 1 1 calc R . .
H68B H 0.2621 0.8903 -0.1374 0.032 Uiso 1 1 calc R . .
C67A C 0.1049(4) 0.6225(9) -0.2190(9) 0.046(2) Uani 0.257(9) 1 d PD A 3
C69 C 0.0677(5) 0.5825(17) -0.1435(14) 0.041(8) Uiso 0.257(9) 1 d PD A 3
H69A H 0.0632 0.6341 -0.0885 0.061 Uiso 0.257(9) 1 calc PR A 3
H69B H 0.0768 0.5153 -0.1134 0.061 Uiso 0.257(9) 1 calc PR A 3
H69C H 0.0397 0.5731 -0.1816 0.061 Uiso 0.257(9) 1 calc PR A 3
C70 C 0.1184(6) 0.5287(12) -0.2909(13) 0.034(7) Uiso 0.257(9) 1 d PD A 3
H70A H 0.0921 0.5040 -0.3284 0.051 Uiso 0.257(9) 1 calc PR A 3
H70B H 0.1305 0.4713 -0.2491 0.051 Uiso 0.257(9) 1 calc PR A 3
H70C H 0.1411 0.5523 -0.3401 0.051 Uiso 0.257(9) 1 calc PR A 3
C71 C 0.0861(7) 0.7147(14) -0.2864(17) 0.077(11) Uiso 0.257(9) 1 d PD A 3
H71A H 0.0753 0.7709 -0.2413 0.116 Uiso 0.257(9) 1 calc PR A 3
H71B H 0.0614 0.6887 -0.3287 0.116 Uiso 0.257(9) 1 calc PR A 3
H71C H 0.1097 0.7419 -0.3311 0.116 Uiso 0.257(9) 1 calc PR A 3
C67B C 0.1005(2) 0.6350(6) -0.2087(5) 0.046(2) Uani 0.743(9) 1 d PD A 4
C72 C 0.0768(4) 0.5384(7) -0.1560(10) 0.096(5) Uani 0.743(9) 1 d PD A 4
H72A H 0.0735 0.5520 -0.0821 0.144 Uiso 0.743(9) 1 calc PR A 4
H72B H 0.0949 0.4752 -0.1662 0.144 Uiso 0.743(9) 1 calc PR A 4
H72C H 0.0474 0.5281 -0.1869 0.144 Uiso 0.743(9) 1 calc PR A 4
C73 C 0.1101(3) 0.6094(13) -0.3244(6) 0.125(7) Uani 0.743(9) 1 d PD A 4
H73A H 0.0819 0.5938 -0.3596 0.188 Uiso 0.743(9) 1 calc PR A 4
H73B H 0.1298 0.5483 -0.3289 0.188 Uiso 0.743(9) 1 calc PR A 4
H73C H 0.1244 0.6699 -0.3572 0.188 Uiso 0.743(9) 1 calc PR A 4
C74 C 0.0683(3) 0.7320(6) -0.2012(9) 0.075(4) Uani 0.743(9) 1 d PD A 4
H74A H 0.0599 0.7434 -0.1291 0.113 Uiso 0.743(9) 1 calc PR A 4
H74B H 0.0414 0.7183 -0.2420 0.113 Uiso 0.743(9) 1 calc PR A 4
H74C H 0.0833 0.7946 -0.2278 0.113 Uiso 0.743(9) 1 calc PR A 4
C81 C 0.09206(18) 0.8311(5) 0.1433(5) 0.0369(16) Uani 1 1 d . . .
C82 C 0.07432(19) 0.9299(5) 0.1746(5) 0.0379(16) Uani 1 1 d . . .
H82 H 0.0940 0.9868 0.1869 0.045 Uiso 1 1 calc R . .
C83 C 0.0276(2) 0.9449(5) 0.1880(5) 0.0421(17) Uani 1 1 d . . .
C84 C -0.0004(2) 0.8586(6) 0.1704(5) 0.0480(19) Uani 1 1 d . . .
H84 H -0.0316 0.8672 0.1796 0.058 Uiso 1 1 calc R . .
C85 C 0.0158(2) 0.7592(6) 0.1394(5) 0.0465(18) Uani 1 1 d . . .
C86 C 0.06220(19) 0.7482(5) 0.1276(5) 0.0417(17) Uani 1 1 d . . .
H44 H 0.0737 0.6816 0.1082 0.050 Uiso 1 1 calc R . .
C87 C 0.14207(16) 0.8157(5) 0.1297(6) 0.0424(15) Uani 1 1 d . . .
H87A H 0.1480 0.7432 0.1086 0.064 Uiso 0.50 1 calc PR . .
H87B H 0.1573 0.8300 0.1950 0.064 Uiso 0.50 1 calc PR . .
H87C H 0.1531 0.8639 0.0767 0.064 Uiso 0.50 1 calc PR . .
H87D H 0.1576 0.8816 0.1450 0.064 Uiso 0.50 1 calc PR . .
H87E H 0.1483 0.7947 0.0586 0.064 Uiso 0.50 1 calc PR . .
H87F H 0.1525 0.7608 0.1768 0.064 Uiso 0.50 1 calc PR . .
C88 C 0.0080(2) 1.0511(5) 0.2223(6) 0.058(2) Uani 1 1 d . . .
H88A H 0.0321 1.1022 0.2305 0.087 Uiso 0.50 1 calc PR . .
H88B H -0.0075 1.0423 0.2882 0.087 Uiso 0.50 1 calc PR . .
H88C H -0.0131 1.0763 0.1702 0.087 Uiso 0.50 1 calc PR . .
H88D H -0.0244 1.0449 0.2288 0.087 Uiso 0.50 1 calc PR . .
H88E H 0.0152 1.1049 0.1711 0.087 Uiso 0.50 1 calc PR . .
H88F H 0.0208 1.0709 0.2890 0.087 Uiso 0.50 1 calc PR . .
C89 C -0.0144(2) 0.6630(6) 0.1221(8) 0.084(3) Uani 1 1 d . . .
H89A H -0.0456 0.6829 0.1335 0.125 Uiso 0.50 1 calc PR . .
H89B H -0.0062 0.6072 0.1705 0.125 Uiso 0.50 1 calc PR . .
H89C H -0.0108 0.6375 0.0514 0.125 Uiso 0.50 1 calc PR . .
H89D H 0.0039 0.6022 0.1034 0.125 Uiso 0.50 1 calc PR . .
H89E H -0.0355 0.6779 0.0664 0.125 Uiso 0.50 1 calc PR . .
H89F H -0.0309 0.6476 0.1855 0.125 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.031(2) 0.029(2) 0.027(2) -0.0048(19) -0.0005(19) 0.0003(18)
O2 0.032(2) 0.038(2) 0.027(2) 0.0058(18) -0.0009(19) 0.0061(19)
O3 0.032(2) 0.033(2) 0.029(2) 0.0049(19) 0.0060(19) -0.0016(19)
O4 0.040(2) 0.028(2) 0.025(2) 0.0066(18) 0.0030(19) 0.011(2)
C1 0.027(3) 0.019(3) 0.021(3) 0.007(3) -0.003(3) 0.009(3)
C2 0.034(3) 0.018(3) 0.020(3) 0.002(3) -0.006(3) 0.008(3)
C3 0.038(3) 0.014(3) 0.035(4) 0.003(3) -0.010(3) 0.000(3)
C4 0.038(3) 0.027(3) 0.021(3) 0.002(3) -0.001(3) 0.003(3)
C5 0.038(3) 0.017(3) 0.021(3) 0.002(3) 0.001(3) 0.007(3)
C6 0.037(3) 0.011(3) 0.026(4) 0.002(3) -0.005(3) 0.003(3)
C8 0.042(3) 0.012(3) 0.032(4) -0.008(3) -0.001(3) 0.006(3)
C7A 0.043(4) 0.042(4) 0.025(4) -0.015(4) 0.009(3) -0.011(3)
C9 0.047(5) 0.054(6) 0.059(6) 0.008(5) 0.016(4) 0.000(4)
C10 0.056(5) 0.037(5) 0.054(6) 0.012(4) 0.016(4) -0.006(4)
C11 0.084(6) 0.119(9) 0.049(6) -0.039(6) 0.026(5) -0.065(7)
C7B 0.043(4) 0.042(4) 0.025(4) -0.015(4) 0.009(3) -0.011(3)
C21 0.028(3) 0.020(3) 0.024(3) -0.001(3) -0.002(3) -0.004(3)
C22 0.032(3) 0.027(3) 0.018(3) -0.005(3) -0.010(3) 0.001(3)
C23 0.045(4) 0.023(3) 0.014(3) 0.003(3) 0.006(3) -0.003(3)
C24 0.033(3) 0.032(3) 0.013(3) 0.001(3) -0.004(3) 0.004(3)
C25 0.029(3) 0.012(3) 0.020(3) 0.001(3) -0.003(3) 0.003(3)
C26 0.030(3) 0.018(3) 0.022(3) 0.010(3) -0.011(3) -0.007(3)
C27 0.044(4) 0.025(3) 0.028(3) 0.006(3) 0.000(3) -0.002(3)
C28 0.045(4) 0.015(3) 0.015(3) 0.002(2) -0.002(3) 0.006(3)
C29 0.056(4) 0.062(5) 0.066(5) 0.025(4) 0.042(4) 0.028(4)
C30 0.054(4) 0.059(4) 0.032(4) -0.006(4) 0.006(3) 0.009(3)
C31 0.043(4) 0.072(5) 0.035(4) -0.005(4) 0.002(3) 0.000(4)
C41 0.028(3) 0.023(3) 0.031(4) 0.005(3) 0.003(3) 0.000(3)
C42 0.031(3) 0.021(3) 0.021(3) 0.002(3) 0.006(3) -0.011(3)
C43 0.039(3) 0.011(3) 0.024(3) -0.002(3) 0.003(3) -0.002(3)
C44 0.030(3) 0.021(3) 0.022(3) -0.003(3) 0.001(3) -0.002(3)
C45 0.035(3) 0.026(3) 0.023(3) 0.006(3) -0.001(3) -0.004(3)
C46 0.041(3) 0.026(3) 0.011(3) 0.006(3) 0.005(3) -0.005(3)
C47 0.052(4) 0.031(4) 0.029(4) 0.004(3) -0.001(3) -0.005(3)
C48 0.029(3) 0.014(3) 0.020(3) -0.002(3) -0.003(3) -0.003(3)
C49 0.046(4) 0.058(5) 0.046(4) 0.006(4) -0.003(4) -0.002(3)
C50 0.051(4) 0.040(4) 0.042(4) 0.005(4) -0.001(3) 0.015(3)
C51 0.052(4) 0.067(5) 0.047(4) -0.004(4) -0.006(4) 0.024(4)
C61 0.019(3) 0.041(4) 0.016(3) -0.002(3) 0.005(3) 0.005(3)
C62 0.044(4) 0.008(3) 0.010(3) 0.000(2) 0.006(3) 0.007(3)
C63 0.050(4) 0.013(3) 0.014(3) 0.007(3) -0.002(3) 0.003(3)
C64 0.054(4) 0.021(3) 0.019(3) 0.004(3) -0.009(3) 0.005(3)
C65 0.047(4) 0.023(3) 0.022(3) -0.007(3) 0.005(3) -0.007(3)
C66 0.037(3) 0.019(3) 0.019(3) -0.014(3) 0.005(3) 0.001(3)
C68 0.034(3) 0.026(3) 0.019(3) 0.005(3) 0.012(3) 0.001(3)
C67A 0.050(4) 0.043(4) 0.045(4) 0.006(4) -0.024(4) -0.006(4)
C67B 0.050(4) 0.043(4) 0.045(4) 0.006(4) -0.024(4) -0.006(4)
C72 0.098(8) 0.030(7) 0.161(13) 0.023(8) -0.077(8) -0.036(6)
C73 0.080(8) 0.24(2) 0.060(8) -0.062(10) -0.032(7) -0.003(11)
C74 0.046(6) 0.051(7) 0.129(11) 0.015(7) -0.036(7) 0.009(5)
C81 0.040(3) 0.040(4) 0.030(4) 0.010(3) -0.001(3) 0.007(3)
C82 0.036(3) 0.047(4) 0.031(4) 0.009(3) -0.005(3) -0.001(3)
C83 0.039(4) 0.051(4) 0.036(4) -0.002(3) -0.001(3) 0.006(3)
C84 0.033(4) 0.078(6) 0.033(4) 0.001(4) 0.000(3) 0.001(4)
C85 0.044(4) 0.056(4) 0.040(4) -0.009(4) -0.006(4) -0.021(4)
C86 0.051(4) 0.035(4) 0.039(4) -0.005(3) -0.003(4) -0.005(3)
C87 0.040(3) 0.033(3) 0.054(4) -0.003(3) 0.004(4) -0.001(3)
C88 0.050(4) 0.054(5) 0.070(5) -0.004(4) 0.008(4) 0.016(4)
C89 0.064(4) 0.072(6) 0.116(7) -0.020(6) -0.013(6) -0.035(5)

_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.397(6) . ?
O2 C21 1.380(6) . ?
O3 C41 1.395(6) . ?
O4 C61 1.390(6) . ?
C1 C2 1.396(7) . ?
C1 C6 1.415(8) . ?
C2 C3 1.388(7) . ?
C2 C8 1.513(8) . ?
C3 C4 1.389(8) . ?
C4 C5 1.374(7) . ?
C4 C7B 1.530(9) . ?
C4 C7A 1.534(6) . ?
C5 C6 1.370(7) . ?
C6 C28 1.523(7) . ?
C8 C66 1.526(8) . ?
C7A C9 1.536(7) . ?
C7A C10 1.541(7) . ?
C7A C11 1.544(7) . ?
C7B C14 1.529(9) . ?
C7B C12 1.530(10) . ?
C7B C13 1.530(9) . ?
C21 C22 1.384(8) . ?
C21 C26 1.409(7) . ?
C22 C23 1.355(7) . ?
C22 C28 1.536(8) . ?
C23 C24 1.404(7) . ?
C24 C25 1.387(7) . ?
C24 C27 1.515(8) . ?
C25 C26 1.376(7) . ?
C26 C48 1.529(7) . ?
C27 C29 1.517(8) . ?
C27 C30 1.526(8) . ?
C27 C31 1.548(8) . ?
C41 C46 1.393(7) . ?
C41 C42 1.397(8) . ?
C42 C43 1.401(7) . ?
C42 C48 1.511(7) . ?
C43 C44 1.375(7) . ?
C44 C45 1.400(7) . ?
C44 C47 1.531(8) . ?
C45 C46 1.382(7) . ?
C46 C68 1.531(7) . ?
C47 C49 1.514(8) . ?
C47 C50 1.532(8) . ?
C47 C51 1.550(9) . ?
C61 C66 1.383(8) . ?
C61 C62 1.413(7) . ?
C62 C63 1.381(8) . ?
C62 C68 1.516(7) . ?
C63 C64 1.383(7) . ?
C64 C65 1.391(7) . ?
C64 C67A 1.540(9) . ?
C64 C67B 1.541(7) . ?
C65 C66 1.388(7) . ?
C67A C71 1.537(9) . ?
C67A C70 1.538(9) . ?
C67A C69 1.541(9) . ?
C67B C73 1.532(8) . ?
C67B C74 1.540(8) . ?
C67B C72 1.545(8) . ?
C81 C86 1.372(8) . ?
C81 C82 1.397(8) . ?
C81 C87 1.493(7) . ?
C82 C83 1.397(8) . ?
C83 C84 1.373(9) . ?
C83 C88 1.510(9) . ?
C84 C85 1.386(9) . ?
C85 C86 1.378(8) . ?
C85 C89 1.512(9) . ?

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
C2 C1 O1 118.4(5) . . ?
C2 C1 C6 121.5(5) . . ?
O1 C1 C6 120.0(5) . . ?
C3 C2 C1 117.1(5) . . ?
C3 C2 C8 121.1(5) . . ?
C1 C2 C8 121.7(5) . . ?
C2 C3 C4 122.9(5) . . ?
C5 C4 C3 117.6(5) . . ?
C5 C4 C7B 131.8(7) . . ?
C3 C4 C7B 110.5(7) . . ?
C5 C4 C7A 117.8(5) . . ?
C3 C4 C7A 124.6(5) . . ?
C7B C4 C7A 14.1(6) . . ?
C6 C5 C4 123.2(5) . . ?
C5 C6 C1 117.5(5) . . ?
C5 C6 C28 120.9(5) . . ?
C1 C6 C28 121.4(5) . . ?
C2 C8 C66 112.4(4) . . ?
C4 C7A C9 110.9(5) . . ?
C4 C7A C10 109.1(5) . . ?
C9 C7A C10 110.0(5) . . ?
C4 C7A C11 111.1(5) . . ?
C9 C7A C11 107.7(6) . . ?
C10 C7A C11 107.9(6) . . ?
C14 C7B C4 111.7(11) . . ?
C14 C7B C12 110.7(11) . . ?
C4 C7B C12 101.3(18) . . ?
C14 C7B C13 111.0(12) . . ?
C4 C7B C13 109.8(11) . . ?
C12 C7B C13 112.1(13) . . ?
O2 C21 C22 118.7(5) . . ?
O2 C21 C26 121.2(5) . . ?
C22 C21 C26 120.1(5) . . ?
C23 C22 C21 119.5(5) . . ?
C23 C22 C28 120.0(5) . . ?
C21 C22 C28 120.3(5) . . ?
C22 C23 C24 122.6(5) . . ?
C25 C24 C23 116.7(5) . . ?
C25 C24 C27 123.7(5) . . ?
C23 C24 C27 119.6(5) . . ?
C26 C25 C24 122.5(5) . . ?
C25 C26 C21 118.5(5) . . ?
C25 C26 C48 120.1(5) . . ?
C21 C26 C48 121.2(5) . . ?
C24 C27 C29 112.1(5) . . ?
C24 C27 C30 109.1(5) . . ?
C29 C27 C30 109.0(5) . . ?
C24 C27 C31 109.7(5) . . ?
C29 C27 C31 108.8(5) . . ?
C30 C27 C31 108.1(5) . . ?
C6 C28 C22 111.5(4) . . ?
C46 C41 O3 121.1(5) . . ?
C46 C41 C42 121.2(5) . . ?
O3 C41 C42 117.7(5) . . ?
C41 C42 C43 117.6(5) . . ?
C41 C42 C48 121.6(5) . . ?
C43 C42 C48 120.8(5) . . ?
C44 C43 C42 123.0(5) . . ?
C43 C44 C45 117.1(5) . . ?
C43 C44 C47 124.5(5) . . ?
C45 C44 C47 118.4(5) . . ?
C46 C45 C44 122.5(5) . . ?
C45 C46 C41 118.5(5) . . ?
C45 C46 C68 119.5(5) . . ?
C41 C46 C68 122.0(5) . . ?
C49 C47 C44 110.4(5) . . ?
C49 C47 C50 108.6(5) . . ?
C44 C47 C50 109.1(5) . . ?
C49 C47 C51 109.3(5) . . ?
C44 C47 C51 111.8(5) . . ?
C50 C47 C51 107.5(5) . . ?
C42 C48 C26 113.8(4) . . ?
C66 C61 O4 122.2(5) . . ?
C66 C61 C62 121.5(5) . . ?
O4 C61 C62 116.3(5) . . ?
C63 C62 C61 117.6(5) . . ?
C63 C62 C68 120.2(5) . . ?
C61 C62 C68 122.2(5) . . ?
C62 C63 C64 123.3(5) . . ?
C63 C64 C65 116.7(5) . . ?
C63 C64 C67A 123.5(6) . . ?
C65 C64 C67A 119.0(6) . . ?
C63 C64 C67B 121.3(5) . . ?
C65 C64 C67B 122.0(5) . . ?
C67A C64 C67B 9.0(6) . . ?
C66 C65 C64 123.3(5) . . ?
C61 C66 C65 117.7(5) . . ?
C61 C66 C8 122.0(5) . . ?
C65 C66 C8 120.2(5) . . ?
C62 C68 C46 111.0(4) . . ?
C71 C67A C70 109.3(10) . . ?
C71 C67A C64 110.0(10) . . ?
C70 C67A C64 111.2(9) . . ?
C71 C67A C69 109.5(11) . . ?
C70 C67A C69 107.9(10) . . ?
C64 C67A C69 109.0(9) . . ?
C73 C67B C74 109.7(8) . . ?
C73 C67B C64 108.7(6) . . ?
C74 C67B C64 109.5(6) . . ?
C73 C67B C72 109.7(8) . . ?
C74 C67B C72 108.0(7) . . ?
C64 C67B C72 111.4(6) . . ?
C86 C81 C82 117.9(5) . . ?
C86 C81 C87 121.1(6) . . ?
C82 C81 C87 121.0(6) . . ?
C81 C82 C83 121.3(6) . . ?
C84 C83 C82 117.7(6) . . ?
C84 C83 C88 120.5(5) . . ?
C82 C83 C88 121.8(6) . . ?
C83 C84 C85 122.7(6) . . ?
C86 C85 C84 117.5(6) . . ?
C86 C85 C89 119.1(6) . . ?
C84 C85 C89 123.3(6) . . ?
C81 C86 C85 122.8(6) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 22.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.245
_refine_diff_density_min -0.255
_refine_diff_density_rms 0.063