#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:39:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179121 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308316.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_4308316
loop_
_publ_author_name
'Geoffroy Guillemot'
'Barbara Castellano'
'Thierry Prangé'
'Euro Solari'
'Carlo Floriani'
_publ_section_title
;
Use of Calix[4]arenes in the Redox Chemistry of Lanthanides: the
Reduction of Dinitrogen by a Calix[4]arene-Samarium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5152
_journal_page_last               5154
_journal_paper_doi               10.1021/ic700787d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C116 H164 Cl2 N0 O14 Sm2'
_chemical_formula_weight         2154.07
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(10)
_cell_angle_beta                 109.004(10)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            4
_cell_length_a                   35.1360(2)
_cell_length_b                   16.7980(2)
_cell_length_c                   20.6270(2)
_cell_measurement_temperature    293(2)
_cell_volume                     11510.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8844
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.114
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4520
_refine_diff_density_max         1.526
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8844
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          1.780
_refine_ls_shift/su_mean         0.091
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0823P)²+191.5356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                6893
_reflns_number_total             8844
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700787d-file003.cif
_cod_data_source_block           gg801
_cod_original_cell_volume        11510.80(19)
_cod_database_code               4308316
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Sm1 Sm 0.055343(15) 0.71403(3) 0.21154(2) 0.03870(19) Uani 1 1 d . . .
Cl2 Cl 0.0000 0.8150(2) 0.2500 0.0469(8) Uani 1 2 d S . .
Cl3 Cl 0.0000 0.6165(2) 0.2500 0.0523(9) Uani 1 2 d S . .
C1 C 0.0615(3) 0.5771(5) 0.0905(4) 0.039(2) Uani 1 1 d . . .
C2 C 0.0312(3) 0.5953(5) 0.0284(5) 0.044(2) Uani 1 1 d . . .
C3 C 0.0432(3) 0.5996(5) -0.0297(5) 0.042(2) Uani 1 1 d . . .
H3 H 0.0242 0.6151 -0.0708 0.050 Uiso 1 1 calc R . .
C4 C 0.0822(3) 0.5817(6) -0.0298(5) 0.047(2) Uani 1 1 d . . .
C5 C 0.1106(3) 0.5614(6) 0.0326(5) 0.047(2) Uani 1 1 d . . .
H5 H 0.1365 0.5479 0.0339 0.057 Uiso 1 1 calc R . .
C6 C 0.1012(3) 0.5608(6) 0.0941(5) 0.044(2) Uani 1 1 d . . .
O1 O 0.05180(19) 0.5754(4) 0.1521(3) 0.0422(15) Uani 1 1 d . . .
C7 C 0.1353(3) 0.5507(6) 0.1620(5) 0.046(2) Uani 1 1 d . . .
H7A H 0.1243 0.5472 0.1994 0.056 Uiso 1 1 calc R . .
H7B H 0.1499 0.5018 0.1611 0.056 Uiso 1 1 calc R . .
C8 C 0.1638(3) 0.6213(6) 0.1731(5) 0.043(2) Uani 1 1 d . . .
C9 C 0.1993(3) 0.6181(6) 0.1562(5) 0.049(2) Uani 1 1 d . . .
H9 H 0.2069 0.5696 0.1424 0.059 Uiso 1 1 calc R . .
C10 C 0.2238(3) 0.6843(7) 0.1590(5) 0.050(2) Uani 1 1 d . . .
C11 C 0.2109(3) 0.7551(7) 0.1800(5) 0.048(2) Uani 1 1 d . . .
H11 H 0.2269 0.8002 0.1839 0.058 Uiso 1 1 calc R . .
C12 C 0.1755(3) 0.7617(6) 0.1952(5) 0.051(3) Uani 1 1 d . . .
C13 C 0.1510(3) 0.6954(6) 0.1929(5) 0.043(2) Uani 1 1 d . . .
O2 O 0.11624(19) 0.6988(4) 0.2075(3) 0.0444(15) Uani 1 1 d . . .
C14 C 0.1606(3) 0.8431(6) 0.2119(5) 0.047(2) Uani 1 1 d . . .
H14A H 0.1506 0.8378 0.2502 0.057 Uiso 1 1 calc R . .
H14B H 0.1828 0.8807 0.2246 0.057 Uiso 1 1 calc R . .
C15 C 0.1275(3) 0.8734(6) 0.1496(5) 0.044(2) Uani 1 1 d . . .
C16 C 0.1369(3) 0.8957(6) 0.0906(5) 0.045(2) Uani 1 1 d . . .
H16 H 0.1637 0.8944 0.0922 0.054 Uiso 1 1 calc R . .
C17 C 0.1076(3) 0.9197(6) 0.0298(5) 0.046(2) Uani 1 1 d . . .
C18 C 0.0679(3) 0.9221(5) 0.0296(5) 0.044(2) Uani 1 1 d . . .
H18 H 0.0480 0.9377 -0.0104 0.053 Uiso 1 1 calc R . .
C19 C 0.0564(3) 0.9024(5) 0.0856(5) 0.041(2) Uani 1 1 d . . .
C20 C 0.0869(3) 0.8789(5) 0.1455(4) 0.038(2) Uani 1 1 d . . .
O3 O 0.07639(19) 0.8572(4) 0.2041(3) 0.0424(15) Uani 1 1 d . . .
C21 C 0.0112(3) 0.9023(6) 0.0786(5) 0.043(2) Uani 1 1 d . . .
H21A H 0.0083 0.8919 0.1229 0.052 Uiso 1 1 calc R . .
H21B H -0.0002 0.9544 0.0633 0.052 Uiso 1 1 calc R . .
C22 C -0.0115(3) 0.8395(5) 0.0276(5) 0.041(2) Uani 1 1 d . . .
C23 C -0.0375(3) 0.8574(6) -0.0372(5) 0.047(2) Uani 1 1 d . . .
H23 H -0.0424 0.9107 -0.0493 0.057 Uiso 1 1 calc R . .
C24 C -0.0566(3) 0.7995(6) -0.0855(5) 0.050(2) Uani 1 1 d . . .
C25 C -0.0494(3) 0.7201(5) -0.0655(5) 0.040(2) Uani 1 1 d . . .
H25 H -0.0624 0.6804 -0.0962 0.048 Uiso 1 1 calc R . .
C26 C -0.0231(3) 0.6981(6) -0.0007(5) 0.043(2) Uani 1 1 d . . .
C27 C -0.0041(3) 0.7601(6) 0.0464(4) 0.040(2) Uani 1 1 d . . .
O4 O 0.02050(19) 0.7400(4) 0.1089(3) 0.0427(15) Uani 1 1 d . . .
C28 C -0.0117(3) 0.6143(5) 0.0229(5) 0.043(2) Uani 1 1 d . . .
H28A H -0.0297 0.5777 -0.0091 0.051 Uiso 1 1 calc R . .
H28B H -0.0152 0.6066 0.0673 0.051 Uiso 1 1 calc R . .
C29 C 0.0950(3) 0.5833(7) -0.0956(5) 0.053(3) Uani 1 1 d . . .
C30 C 0.1352(4) 0.6272(9) -0.0813(6) 0.084(4) Uani 1 1 d . . .
H30A H 0.1322 0.6813 -0.0689 0.125 Uiso 1 1 calc R . .
H30B H 0.1431 0.6263 -0.1217 0.125 Uiso 1 1 calc R . .
H30C H 0.1554 0.6013 -0.0443 0.125 Uiso 1 1 calc R . .
C31 C 0.0618(4) 0.6231(8) -0.1553(5) 0.067(3) Uani 1 1 d . . .
H31A H 0.0583 0.6773 -0.1435 0.101 Uiso 1 1 calc R . .
H31B H 0.0370 0.5946 -0.1636 0.101 Uiso 1 1 calc R . .
H31C H 0.0695 0.6221 -0.1959 0.101 Uiso 1 1 calc R . .
C32 C 0.1002(4) 0.4976(7) -0.1149(6) 0.077(4) Uani 1 1 d . . .
H32A H 0.0752 0.4697 -0.1242 0.116 Uiso 1 1 calc R . .
H32B H 0.1205 0.4721 -0.0778 0.116 Uiso 1 1 calc R . .
H32C H 0.1083 0.4969 -0.1551 0.116 Uiso 1 1 calc R . .
C33 C 0.2612(3) 0.6764(7) 0.1348(5) 0.056(3) Uani 1 1 d . . .
C34 C 0.2472(4) 0.6493(9) 0.0592(6) 0.074(4) Uani 1 1 d . . .
H34A H 0.2327 0.6000 0.0548 0.111 Uiso 1 1 calc R . .
H34B H 0.2702 0.6417 0.0445 0.111 Uiso 1 1 calc R . .
H34C H 0.2300 0.6891 0.0311 0.111 Uiso 1 1 calc R . .
C35 C 0.2840(4) 0.7548(9) 0.1403(7) 0.078(4) Uani 1 1 d . . .
H35A H 0.2930 0.7724 0.1871 0.118 Uiso 1 1 calc R . .
H35B H 0.2665 0.7942 0.1121 0.118 Uiso 1 1 calc R . .
H35C H 0.3068 0.7471 0.1252 0.118 Uiso 1 1 calc R . .
C36 C 0.2905(4) 0.6139(8) 0.1796(6) 0.073(4) Uani 1 1 d . . .
H36A H 0.2768 0.5640 0.1770 0.110 Uiso 1 1 calc R . .
H36B H 0.3000 0.6318 0.2264 0.110 Uiso 1 1 calc R . .
H36C H 0.3130 0.6073 0.1634 0.110 Uiso 1 1 calc R . .
C37 C 0.1195(4) 0.9393(7) -0.0343(6) 0.061(3) Uani 1 1 d . . .
C38 C 0.1309(6) 0.8588(12) -0.0617(9) 0.132(7) Uani 1 1 d . . .
H38A H 0.1083 0.8233 -0.0731 0.198 Uiso 1 1 calc R . .
H38B H 0.1532 0.8349 -0.0270 0.198 Uiso 1 1 calc R . .
H38C H 0.1383 0.8688 -0.1019 0.198 Uiso 1 1 calc R . .
C39 C 0.1560(6) 0.9860(14) -0.0187(9) 0.159(10) Uani 1 1 d . . .
H39A H 0.1765 0.9626 0.0194 0.239 Uiso 1 1 calc R . .
H39B H 0.1508 1.0394 -0.0073 0.239 Uiso 1 1 calc R . .
H39C H 0.1650 0.9869 -0.0580 0.239 Uiso 1 1 calc R . .
C40 C 0.0852(5) 0.9669(16) -0.0929(8) 0.163(11) Uani 1 1 d . . .
H40A H 0.0628 0.9316 -0.0993 0.245 Uiso 1 1 calc R . .
H40B H 0.0927 0.9672 -0.1336 0.245 Uiso 1 1 calc R . .
H40C H 0.0777 1.0197 -0.0839 0.245 Uiso 1 1 calc R . .
C41 C -0.0834(4) 0.8237(7) -0.1577(5) 0.062(3) Uani 1 1 d . . .
C42 C -0.1071(5) 0.7525(8) -0.1995(7) 0.093(5) Uani 1 1 d . . .
H42A H -0.1235 0.7706 -0.2439 0.139 Uiso 1 1 calc R . .
H42B H -0.1240 0.7298 -0.1758 0.139 Uiso 1 1 calc R . .
H42C H -0.0886 0.7130 -0.2045 0.139 Uiso 1 1 calc R . .
C43 C -0.1141(4) 0.8862(8) -0.1530(7) 0.092(5) Uani 1 1 d . . .
H43A H -0.1002 0.9310 -0.1270 0.137 Uiso 1 1 calc R . .
H43B H -0.1317 0.8635 -0.1309 0.137 Uiso 1 1 calc R . .
H43C H -0.1296 0.9034 -0.1983 0.137 Uiso 1 1 calc R . .
C44 C -0.0559(5) 0.8603(10) -0.1959(6) 0.101(5) Uani 1 1 d . . .
H44A H -0.0412 0.9044 -0.1700 0.151 Uiso 1 1 calc R . .
H44B H -0.0722 0.8784 -0.2404 0.151 Uiso 1 1 calc R . .
H44C H -0.0373 0.8206 -0.2007 0.151 Uiso 1 1 calc R . .
ME1 C 0.0441(3) 0.4960(5) 0.1707(5) 0.048(2) Uani 1 1 d . . .
HE1A H 0.0377 0.4977 0.2125 0.073 Uiso 1 1 calc R . .
HE1B H 0.0676 0.4638 0.1772 0.073 Uiso 1 1 calc R . .
HE1C H 0.0219 0.4737 0.1349 0.073 Uiso 1 1 calc R . .
ME3 C 0.0796(4) 0.9221(6) 0.2512(5) 0.057(3) Uani 1 1 d . . .
HE3A H 0.0722 0.9039 0.2896 0.085 Uiso 1 1 calc R . .
HE3B H 0.0620 0.9644 0.2284 0.085 Uiso 1 1 calc R . .
HE3C H 0.1069 0.9412 0.2670 0.085 Uiso 1 1 calc R . .
O1_1 O 0.09511(19) 0.7251(5) 0.3362(3) 0.0579(19) Uani 1 1 d D . .
C2_1 C 0.1386(3) 0.7202(8) 0.3651(6) 0.067(3) Uani 1 1 d D . .
H21_1 H 0.1512 0.7456 0.3350 0.080 Uiso 1 1 calc R . .
H22_1 H 0.1472 0.6650 0.3714 0.080 Uiso 1 1 calc R . .
C3_1 C 0.1499(4) 0.7628(15) 0.4334(8) 0.148(10) Uani 1 1 d D . .
H31_1 H 0.1546 0.8190 0.4285 0.178 Uiso 1 1 calc R . .
H32_1 H 0.1736 0.7394 0.4663 0.178 Uiso 1 1 calc R . .
C4_1 C 0.1118(4) 0.7492(17) 0.4547(7) 0.160(11) Uani 1 1 d D . .
H41_1 H 0.1152 0.7024 0.4836 0.192 Uiso 1 1 calc R . .
H42_1 H 0.1071 0.7948 0.4798 0.192 Uiso 1 1 calc R . .
C5_1 C 0.0780(3) 0.7380(8) 0.3907(5) 0.060(3) Uani 1 1 d D . .
H51_1 H 0.0620 0.6924 0.3947 0.072 Uiso 1 1 calc R . .
H52_1 H 0.0609 0.7848 0.3810 0.072 Uiso 1 1 calc R . .
O1_2 O 0.2467(7) 0.9545(10) 0.1428(12) 0.231(9) Uani 1 1 d D . .
C2_2 C 0.2366(7) 1.0171(12) 0.1775(10) 0.162(10) Uani 1 1 d D . .
H21_2 H 0.2520 1.0136 0.2259 0.195 Uiso 1 1 calc R . .
H22_2 H 0.2083 1.0140 0.1726 0.195 Uiso 1 1 calc R . .
C3_2 C 0.2453(7) 1.0961(11) 0.1492(11) 0.137(7) Uani 1 1 d D . .
H31_2 H 0.2580 1.1329 0.1861 0.164 Uiso 1 1 calc R . .
H32_2 H 0.2206 1.1199 0.1193 0.164 Uiso 1 1 calc R . .
C4_2 C 0.2743(13) 1.0747(17) 0.108(2) 0.40(4) Uani 1 1 d D . .
H41_2 H 0.2610 1.0768 0.0590 0.482 Uiso 1 1 calc R . .
H42_2 H 0.2981 1.1080 0.1208 0.482 Uiso 1 1 calc R . .
C5_2 C 0.2839(7) 0.987(2) 0.1349(18) 0.31(3) Uani 1 1 d D . .
H51_2 H 0.2922 0.9558 0.1024 0.375 Uiso 1 1 calc R . .
H52_2 H 0.3055 0.9869 0.1786 0.375 Uiso 1 1 calc R . .
O1_3 O 0.2526(6) 0.3050(18) 0.1129(14) 0.315(18) Uani 1 1 d D . .
C2_3 C 0.2152(8) 0.2914(14) 0.1299(13) 0.193(13) Uani 1 1 d D . .
H21_3 H 0.1986 0.2507 0.1007 0.231 Uiso 1 1 calc R . .
H21_3 H 0.2212 0.2757 0.1774 0.231 Uiso 1 1 calc R . .
C3_3 C 0.1949(9) 0.3710(14) 0.1166(17) 0.244(18) Uani 1 1 d D . .
H31_3 H 0.2031 0.4036 0.1577 0.292 Uiso 1 1 calc R . .
H32_3 H 0.1658 0.3650 0.1016 0.292 Uiso 1 1 calc R . .
C4_3 C 0.2082(7) 0.4082(13) 0.0607(14) 0.189(12) Uani 1 1 d D . .
H41_3 H 0.2073 0.4658 0.0625 0.227 Uiso 1 1 calc R . .
H42_3 H 0.1915 0.3905 0.0157 0.227 Uiso 1 1 calc R . .
C5_3 C 0.2514(9) 0.3783(18) 0.077(2) 0.29(2) Uani 1 1 d D . .
H51_3 H 0.2579 0.3698 0.0354 0.347 Uiso 1 1 calc R . .
H52_3 H 0.2703 0.4163 0.1057 0.347 Uiso 1 1 calc R . .
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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
O4 Sm1 O2 103.9(2) . . ?
O4 Sm1 O1_1 163.7(3) . . ?
O2 Sm1 O1_1 79.7(2) . . ?
O4 Sm1 O3 80.1(2) . . ?
O2 Sm1 O3 78.5(2) . . ?
O1_1 Sm1 O3 85.2(2) . . ?
O4 Sm1 O1 77.9(2) . . ?
O2 Sm1 O1 77.0(2) . . ?
O1_1 Sm1 O1 118.3(2) . . ?
O3 Sm1 O1 141.82(18) . . ?
O4 Sm1 Cl3 99.93(17) . . ?
O2 Sm1 Cl3 135.27(18) . . ?
O1_1 Sm1 Cl3 87.71(16) . . ?
O3 Sm1 Cl3 143.33(15) . . ?
O1 Sm1 Cl3 71.70(14) . . ?
O4 Sm1 Cl2 86.09(16) . . ?
O2 Sm1 Cl2 146.91(17) . . ?
O1_1 Sm1 Cl2 82.78(16) . . ?
O3 Sm1 Cl2 72.22(15) . . ?
O1 Sm1 Cl2 136.07(15) . . ?
Cl3 Sm1 Cl2 71.21(8) . . ?
Sm1 Cl2 Sm1 107.84(11) 2 . ?
Sm1 Cl3 Sm1 109.73(12) 2 . ?
C6 C1 C2 122.4(8) . . ?
C6 C1 O1 118.4(8) . . ?
C2 C1 O1 119.2(8) . . ?
C3 C2 C1 116.2(9) . . ?
C3 C2 C28 119.9(9) . . ?
C1 C2 C28 123.8(8) . . ?
C2 C3 C4 123.9(9) . . ?
C5 C4 C3 117.3(9) . . ?
C5 C4 C29 119.0(9) . . ?
C3 C4 C29 123.7(9) . . ?
C4 C5 C6 121.7(9) . . ?
C1 C6 C5 118.3(9) . . ?
C1 C6 C7 122.8(8) . . ?
C5 C6 C7 118.7(9) . . ?
C1 O1 ME1 112.2(7) . . ?
C1 O1 Sm1 114.5(5) . . ?
ME1 O1 Sm1 133.2(5) . . ?
C8 C7 C6 109.5(8) . . ?
C9 C8 C13 119.5(9) . . ?
C9 C8 C7 121.9(9) . . ?
C13 C8 C7 118.2(8) . . ?
C10 C9 C8 123.1(10) . . ?
C11 C10 C9 115.9(9) . . ?
C11 C10 C33 124.4(10) . . ?
C9 C10 C33 119.5(10) . . ?
C12 C11 C10 123.1(10) . . ?
C11 C12 C13 121.1(10) . . ?
C11 C12 C14 121.0(9) . . ?
C13 C12 C14 117.8(9) . . ?
O2 C13 C12 123.3(9) . . ?
O2 C13 C8 119.4(8) . . ?
C12 C13 C8 117.3(9) . . ?
C13 O2 Sm1 169.1(6) . . ?
C15 C14 C12 109.4(8) . . ?
C20 C15 C16 116.7(9) . . ?
C20 C15 C14 124.0(8) . . ?
C16 C15 C14 119.3(9) . . ?
C17 C16 C15 122.5(9) . . ?
C18 C17 C16 117.1(9) . . ?
C18 C17 C37 122.7(9) . . ?
C16 C17 C37 120.1(9) . . ?
C19 C18 C17 123.7(9) . . ?
C18 C19 C20 117.2(9) . . ?
C18 C19 C21 119.4(8) . . ?
C20 C19 C21 123.3(8) . . ?
C19 C20 C15 122.8(8) . . ?
C19 C20 O3 119.1(8) . . ?
C15 C20 O3 118.1(8) . . ?
C20 O3 ME3 113.2(7) . . ?
C20 O3 Sm1 117.2(5) . . ?
ME3 O3 Sm1 129.6(5) . . ?
C22 C21 C19 110.9(7) . . ?
C23 C22 C27 118.9(9) . . ?
C23 C22 C21 123.3(9) . . ?
C27 C22 C21 117.8(8) . . ?
C22 C23 C24 123.3(9) . . ?
C25 C24 C23 117.1(9) . . ?
C25 C24 C41 122.4(9) . . ?
C23 C24 C41 120.5(9) . . ?
C24 C25 C26 122.2(9) . . ?
C25 C26 C27 118.2(8) . . ?
C25 C26 C28 125.3(8) . . ?
C27 C26 C28 116.5(8) . . ?
O4 C27 C22 120.8(8) . . ?
O4 C27 C26 118.8(8) . . ?
C22 C27 C26 120.3(8) . . ?
C27 O4 Sm1 174.3(6) . . ?
C26 C28 C2 112.2(8) . . ?
C32 C29 C30 108.9(11) . . ?
C32 C29 C31 108.9(10) . . ?
C30 C29 C31 110.8(10) . . ?
C32 C29 C4 107.7(9) . . ?
C30 C29 C4 110.4(8) . . ?
C31 C29 C4 110.0(9) . . ?
C35 C33 C34 108.5(9) . . ?
C35 C33 C36 108.0(10) . . ?
C34 C33 C36 109.6(10) . . ?
C35 C33 C10 112.4(10) . . ?
C34 C33 C10 108.9(9) . . ?
C36 C33 C10 109.4(8) . . ?
C39 C37 C40 116.1(14) . . ?
C39 C37 C17 113.1(11) . . ?
C40 C37 C17 113.0(10) . . ?
C39 C37 C38 103.5(14) . . ?
C40 C37 C38 102.2(15) . . ?
C17 C37 C38 107.3(10) . . ?
C43 C41 C24 110.0(9) . . ?
C43 C41 C42 107.7(11) . . ?
C24 C41 C42 112.5(9) . . ?
C43 C41 C44 109.0(11) . . ?
C24 C41 C44 108.0(10) . . ?
C42 C41 C44 109.5(11) . . ?
C2_1 O1_1 C5_1 109.6(7) . . ?
C2_1 O1_1 Sm1 125.4(6) . . ?
C5_1 O1_1 Sm1 125.0(5) . . ?
O1_1 C2_1 C3_1 106.2(9) . . ?
C2_1 C3_1 C4_1 101.8(10) . . ?
C5_1 C4_1 C3_1 106.5(10) . . ?
O1_1 C5_1 C4_1 107.2(8) . . ?
C2_2 O1_2 C5_2 99.1(16) . . ?
O1_2 C2_2 C3_2 110.4(14) . . ?
C2_2 C3_2 C4_2 104.7(14) . . ?
C5_2 C4_2 C3_2 97.4(15) . . ?
O1_2 C5_2 C4_2 107.0(16) . . ?
C5_3 O1_3 C2_3 112.0(16) . . ?
C3_3 C2_3 O1_3 103.0(16) . . ?
C2_3 C3_3 C4_3 105.1(13) . . ?
C3_3 C4_3 C5_3 103.1(16) . . ?
O1_3 C5_3 C4_3 105.1(15) . . ?
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
Sm1 O4 2.118(6) . ?
Sm1 O2 2.184(6) . ?
Sm1 O1_1 2.501(6) . ?
Sm1 O3 2.536(6) . ?
Sm1 O1 2.616(6) . ?
Sm1 Cl3 2.846(2) . ?
Sm1 Cl2 2.879(2) . ?
Cl2 Sm1 2.879(2) 2 ?
Cl3 Sm1 2.845(2) 2 ?
C1 C6 1.398(13) . ?
C1 C2 1.407(13) . ?
C1 O1 1.419(10) . ?
C2 C3 1.396(12) . ?
C2 C28 1.510(13) . ?
C3 C4 1.403(14) . ?
C4 C5 1.390(14) . ?
C4 C29 1.564(13) . ?
C5 C6 1.411(13) . ?
C6 C7 1.528(13) . ?
O1 ME1 1.438(11) . ?
C7 C8 1.520(13) . ?
C8 C9 1.402(13) . ?
C8 C13 1.427(13) . ?
C9 C10 1.394(14) . ?
C10 C11 1.390(15) . ?
C10 C33 1.559(14) . ?
C11 C12 1.385(14) . ?
C12 C13 1.396(14) . ?
C12 C14 1.542(14) . ?
C13 O2 1.352(11) . ?
C14 C15 1.513(13) . ?
C15 C20 1.405(13) . ?
C15 C16 1.413(13) . ?
C16 C17 1.399(14) . ?
C17 C18 1.393(14) . ?
C17 C37 1.547(13) . ?
C18 C19 1.382(13) . ?
C19 C20 1.400(13) . ?
C19 C21 1.547(13) . ?
C20 O3 1.421(10) . ?
O3 ME3 1.440(11) . ?
C21 C22 1.520(13) . ?
C22 C23 1.384(13) . ?
C22 C27 1.390(13) . ?
C23 C24 1.399(14) . ?
C24 C25 1.394(13) . ?
C24 C41 1.535(14) . ?
C25 C26 1.404(13) . ?
C26 C27 1.431(13) . ?
C26 C28 1.501(13) . ?
C27 O4 1.340(11) . ?
C29 C32 1.521(16) . ?
C29 C30 1.532(15) . ?
C29 C31 1.547(15) . ?
C33 C35 1.526(18) . ?
C33 C34 1.544(15) . ?
C33 C36 1.549(15) . ?
C37 C39 1.45(2) . ?
C37 C40 1.477(19) . ?
C37 C38 1.57(2) . ?
C41 C43 1.529(17) . ?
C41 C42 1.548(16) . ?
C41 C44 1.558(18) . ?
O1_1 C2_1 1.450(11) . ?
O1_1 C5_1 1.454(10) . ?
C2_1 C3_1 1.514(13) . ?
C3_1 C4_1 1.554(14) . ?
C4_1 C5_1 1.473(13) . ?
O1_2 C2_2 1.381(15) . ?
O1_2 C5_2 1.474(17) . ?
C2_2 C3_2 1.519(16) . ?
C3_2 C4_2 1.565(18) . ?
C4_2 C5_2 1.565(19) . ?
O1_3 C5_3 1.427(17) . ?
O1_3 C2_3 1.487(17) . ?
C2_3 C3_3 1.499(17) . ?
C3_3 C4_3 1.514(17) . ?
C4_3 C5_3 1.528(17) . ?
