#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:45:41 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042222.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_7042222
loop_
_publ_author_name
'Li, Ning'
'García-Rodríguez, Raúl'
'Matthews, Peter D.'
'Luo, He-Kuan'
'Wright, Dominic S.'
_publ_section_title
;
 Synthesis, structure and paramagnetic NMR analysis of a series of
 lanthanide-containing [LnTi6O3(O(i)Pr)9(salicylate)6] cages.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4287
_journal_page_last               4295
_journal_paper_doi               10.1039/c7dt00049a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C69 H87 O30 Sm Ti6'
_chemical_formula_sum            'C69 H87 O30 Sm Ti6'
_chemical_formula_weight         1834.13
_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_Hall           'P -6'
_space_group_name_H-M_alt        'P -6'
_symmetry_space_group_name_Hall  'P -6'
_symmetry_space_group_name_H-M   'P -6'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.9683(4)
_cell_length_b                   14.9683(4)
_cell_length_c                   23.6974(9)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.6
_cell_measurement_theta_min      3.41
_cell_volume                     4598.1(2)
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_collection       'Bruker software package, narrow-frames'
_computing_data_reduction
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.858
_diffrn_reflns_theta_max         66.858
_diffrn_reflns_theta_min         3.409
_exptl_absorpt_coefficient_mu    9.516
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (SADABS) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.791
_refine_diff_density_max         3.028
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2572 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0597P)²+4.3518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5380
_reflns_number_total             5582
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00049a2.cif
_cod_data_source_block           sm_b_sq
_cod_depositor_comments
'Adding full bibliography for 7042216--7042227.cif.'
_cod_original_cell_volume        4598.1(3)
_cod_database_code               7042222
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.240
_shelx_estimated_absorpt_t_max   0.349
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.666667 0.333333 0.500000 0.0221(3) Uani 1 6 d S T P . .
Sm2 Sm 1.000000 1.000000 1.000000 0.0248(3) Uani 1 6 d S T P . .
Ti1 Ti 0.46690(14) 0.36487(14) 0.56302(7) 0.0321(4) Uani 1 1 d . . . . .
Ti2 Ti 0.81234(15) 0.76152(15) 0.93691(7) 0.0361(4) Uani 1 1 d . . . . .
O1 O 0.5014(7) 0.3097(7) 0.500000 0.0258(18) Uani 1 2 d S TU P . .
O2 O 0.4860(7) 0.4616(7) 0.500000 0.036(2) Uani 1 2 d S TU P C .
O3 O 0.3302(5) 0.2961(6) 0.5644(3) 0.0465(18) Uani 1 1 d D U . . .
O4 O 0.4811(5) 0.4548(6) 0.6223(3) 0.0448(18) Uani 1 1 d . U . . .
O5 O 0.4712(6) 0.2595(5) 0.6140(3) 0.0389(18) Uani 1 1 d . U . . .
O6 O 0.6325(5) 0.4353(5) 0.5746(2) 0.0295(13) Uani 1 1 d . U . . .
O21 O 0.8360(8) 0.8502(8) 1.000000 0.036(2) Uani 1 2 d S TU P . .
O22 O 0.8379(10) 0.6884(7) 1.000000 0.044(2) Uani 1 2 d S TU P G .
O23 O 0.6756(6) 0.6821(6) 0.9354(3) 0.0465(19) Uani 1 1 d D U . . .
O24 O 0.8346(7) 0.6932(5) 0.8771(3) 0.0486(19) Uani 1 1 d . U . . .
O25 O 0.9785(5) 0.8669(5) 0.9253(3) 0.0336(15) Uani 1 1 d . U . . .
O26 O 0.8065(7) 0.8671(7) 0.8863(4) 0.044(2) Uani 1 1 d . U . . .
C2 C 0.4822(14) 0.5579(12) 0.500000 0.061(5) Uani 1 2 d S TU P . .
H2A H 0.473309 0.558435 0.541798 0.073 Uiso 0.5 1 calc R U P A -1
C2A C 0.5856(19) 0.6471(17) 0.500000 0.088(7) Uani 1 2 d S TU P C .
H2AA H 0.581326 0.710358 0.500000 0.132 Uiso 0.5 1 calc R U P B -1
H2AB H 0.622639 0.645616 0.533766 0.132 Uiso 0.5 1 calc R U P B -1
H2AC H 0.622639 0.645616 0.466234 0.132 Uiso 0.5 1 calc R U P B -1
C2B C 0.372(3) 0.539(3) 0.4861(19) 0.110(16) Uani 0.5 1 d . U P C -1
H2BA H 0.321310 0.465384 0.491486 0.165 Uiso 0.5 1 calc R U P C -1
H2BB H 0.355377 0.580347 0.511160 0.165 Uiso 0.5 1 calc R U P C -1
H2BC H 0.369736 0.557846 0.446760 0.165 Uiso 0.5 1 calc R U P C -1
C3 C 0.2498(16) 0.2532(16) 0.6063(10) 0.066(5) Uiso 0.553(16) 1 d D U P D 1
H3 H 0.282872 0.258896 0.643807 0.079 Uiso 0.553(16) 1 calc R U P D 1
C3A C 0.195(2) 0.311(2) 0.6094(13) 0.083(5) Uiso 0.553(16) 1 d D U P D 1
H3AA H 0.244884 0.383633 0.617220 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3AB H 0.160960 0.305373 0.573319 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3AC H 0.143997 0.282790 0.639615 0.125 Uiso 0.553(16) 1 calc R U P D 1
C3B C 0.182(2) 0.1466(17) 0.5950(13) 0.083(5) Uiso 0.553(16) 1 d D U P D 1
H3BA H 0.127766 0.117483 0.623490 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3BB H 0.151700 0.138617 0.557493 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3BC H 0.221661 0.110196 0.596122 0.125 Uiso 0.553(16) 1 calc R U P D 1
C3' C 0.2268(17) 0.2242(18) 0.5614(13) 0.066(5) Uiso 0.447(16) 1 d D U P D 2
H3A' H 0.208202 0.234349 0.522319 0.079 Uiso 0.447(16) 1 calc R U P D 2
C3A' C 0.167(2) 0.254(3) 0.5963(15) 0.083(5) Uiso 0.447(16) 1 d D U P D 2
H3AD H 0.093496 0.201996 0.593498 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3AE H 0.189199 0.260120 0.635662 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3AF H 0.176909 0.320891 0.583424 0.125 Uiso 0.447(16) 1 calc R U P D 2
C3B' C 0.194(3) 0.1194(18) 0.5622(16) 0.083(5) Uiso 0.447(16) 1 d D U P D 2
H3BD H 0.119028 0.079433 0.559756 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3BE H 0.224538 0.102593 0.530091 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3BF H 0.216986 0.102501 0.597457 0.125 Uiso 0.447(16) 1 calc R U P D 2
C11 C 0.5538(9) 0.5287(8) 0.6547(5) 0.045(3) Uani 1 1 d . U . . .
C12 C 0.5263(11) 0.5790(10) 0.6938(5) 0.059(4) Uani 1 1 d . U . . .
H12A H 0.456351 0.562361 0.696506 0.071 Uiso 1 1 calc R U . . .
C13 C 0.5975(13) 0.6514(14) 0.7282(6) 0.077(4) Uani 1 1 d . U . . .
H13A H 0.576514 0.685952 0.753943 0.092 Uiso 1 1 calc R U . . .
C14 C 0.6959(14) 0.6761(14) 0.7273(6) 0.077(4) Uani 1 1 d . U . . .
H14A H 0.743758 0.726579 0.752586 0.092 Uiso 1 1 calc R U . . .
C15 C 0.7288(11) 0.6274(11) 0.6890(5) 0.060(3) Uani 1 1 d . U . . .
H15A H 0.799103 0.644707 0.688160 0.072 Uiso 1 1 calc R U . . .
C16 C 0.6574(9) 0.5529(9) 0.6519(5) 0.043(3) Uani 1 1 d . U . . .
C17 C 0.4979(9) 0.1915(9) 0.6112(5) 0.040(3) Uani 1 1 d . U . . .
C22 C 0.8406(19) 0.5929(18) 1.000000 0.075(6) Uani 1 2 d S TU P . .
H22' H 0.824150 0.573360 0.959401 0.090 Uiso 0.5 1 calc R U P E -1
C22A C 0.954(3) 0.625(3) 1.000000 0.175(16) Uani 1 2 d S TU P G .
H22A H 0.992764 0.686902 0.976989 0.263 Uiso 0.5 1 calc R U P F -1
H22B H 0.980461 0.638890 1.038764 0.263 Uiso 0.5 1 calc R U P F -1
H22C H 0.962489 0.568753 0.984248 0.263 Uiso 0.5 1 calc R U P F -1
C22B C 0.750(3) 0.510(2) 1.0256(13) 0.098(10) Uani 0.5 1 d . U P G -1
H22D H 0.753714 0.447077 1.024921 0.147 Uiso 0.5 1 calc R U P G -1
H22E H 0.744376 0.528417 1.064708 0.147 Uiso 0.5 1 calc R U P G -1
H22F H 0.688510 0.499304 1.004491 0.147 Uiso 0.5 1 calc R U P G -1
C23 C 0.6031(19) 0.6392(19) 0.8880(11) 0.075(6) Uiso 0.508(14) 1 d D U P H 1
H23A H 0.639309 0.672897 0.852049 0.091 Uiso 0.508(14) 1 calc R U P H 1
C23A C 0.516(3) 0.656(3) 0.8963(14) 0.086(5) Uiso 0.508(14) 1 d D U P H 1
H23B H 0.468394 0.626878 0.864356 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23C H 0.479921 0.621916 0.931251 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23D H 0.541079 0.730044 0.898971 0.129 Uiso 0.508(14) 1 calc R U P H 1
C23B C 0.564(3) 0.528(2) 0.8847(14) 0.086(5) Uiso 0.508(14) 1 d D U P H 1
H23E H 0.622054 0.515370 0.879114 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23F H 0.528375 0.494595 0.919900 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23G H 0.516022 0.498251 0.852995 0.129 Uiso 0.508(14) 1 calc R U P H 1
C23' C 0.5656(18) 0.635(2) 0.9380(12) 0.075(6) Uiso 0.492(14) 1 d D U P H 2
H23H H 0.539457 0.595575 0.974082 0.091 Uiso 0.492(14) 1 calc R U P H 2
C23C C 0.555(3) 0.719(2) 0.9388(14) 0.086(5) Uiso 0.492(14) 1 d D U P H 2
H23I H 0.481495 0.697986 0.940559 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23J H 0.590331 0.761395 0.971925 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23K H 0.585178 0.759885 0.904455 0.129 Uiso 0.492(14) 1 calc R U P H 2
C23D C 0.513(3) 0.568(2) 0.8905(13) 0.086(5) Uiso 0.492(14) 1 d D U P H 2
H23L H 0.522650 0.508108 0.891565 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23M H 0.439166 0.545111 0.892608 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23N H 0.541412 0.606192 0.855288 0.129 Uiso 0.492(14) 1 calc R U P H 2
C31 C 0.9090(10) 0.7003(9) 0.8437(5) 0.048(3) Uani 1 1 d . U . . .
C32 C 0.8870(12) 0.6242(11) 0.8036(6) 0.066(4) Uani 1 1 d . U . . .
H32A H 0.819681 0.565515 0.802020 0.079 Uiso 1 1 calc R U . . .
C33 C 0.9612(15) 0.6325(13) 0.7662(6) 0.081(5) Uani 1 1 d . U . . .
H33A H 0.943174 0.581465 0.737801 0.097 Uiso 1 1 calc R U . . .
C34 C 1.0608(14) 0.7132(13) 0.7692(6) 0.083(5) Uani 1 1 d . U . . .
H34A H 1.111951 0.717694 0.743754 0.100 Uiso 1 1 calc R U . . .
C35 C 1.0856(12) 0.7891(11) 0.8109(5) 0.062(4) Uani 1 1 d . U . . .
H35A H 1.154293 0.845185 0.813581 0.074 Uiso 1 1 calc R U . . .
C36 C 1.0110(9) 0.7835(9) 0.8482(5) 0.044(3) Uani 1 1 d . U . . .
C37 C 0.8261(9) 0.9590(9) 0.8892(5) 0.035(2) Uani 1 1 d . U . . .
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'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 '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
O1 Sm1 O1 120.000(1) 2_655 .
O1 Sm1 O1 120.000(2) 2_655 3_665
O1 Sm1 O1 120.000(1) . 3_665
O1 Sm1 O6 135.73(14) 2_655 .
O1 Sm1 O6 64.7(2) . .
O1 Sm1 O6 73.2(2) 3_665 .
O1 Sm1 O6 73.2(2) 2_655 3_665
O1 Sm1 O6 135.73(14) . 3_665
O1 Sm1 O6 64.7(2) 3_665 3_665
O6 Sm1 O6 77.2(2) . 3_665
O1 Sm1 O6 64.7(2) 2_655 5_656
O1 Sm1 O6 73.2(2) . 5_656
O1 Sm1 O6 135.73(14) 3_665 5_656
O6 Sm1 O6 137.77(10) . 5_656
O6 Sm1 O6 137.77(10) 3_665 5_656
O1 Sm1 O6 73.2(2) 2_655 6_666
O1 Sm1 O6 135.73(14) . 6_666
O1 Sm1 O6 64.7(2) 3_665 6_666
O6 Sm1 O6 137.77(11) . 6_666
O6 Sm1 O6 87.8(3) 3_665 6_666
O6 Sm1 O6 77.2(2) 5_656 6_666
O1 Sm1 O6 64.7(2) 2_655 2_655
O1 Sm1 O6 73.2(2) . 2_655
O1 Sm1 O6 135.73(14) 3_665 2_655
O6 Sm1 O6 77.2(2) . 2_655
O6 Sm1 O6 77.2(2) 3_665 2_655
O6 Sm1 O6 87.8(3) 5_656 2_655
O6 Sm1 O6 137.77(10) 6_666 2_655
O1 Sm1 O6 135.73(14) 2_655 4_556
O1 Sm1 O6 64.7(2) . 4_556
O1 Sm1 O6 73.2(2) 3_665 4_556
O6 Sm1 O6 87.8(3) . 4_556
O6 Sm1 O6 137.77(11) 3_665 4_556
O6 Sm1 O6 77.2(2) 5_656 4_556
O6 Sm1 O6 77.2(2) 6_666 4_556
O6 Sm1 O6 137.77(11) 2_655 4_556
O1 Sm1 Ti1 129.85(19) 2_655 4_556
O1 Sm1 Ti1 28.54(11) . 4_556
O1 Sm1 Ti1 103.8(2) 3_665 4_556
O6 Sm1 Ti1 77.24(14) . 4_556
O6 Sm1 Ti1 154.15(14) 3_665 4_556
O6 Sm1 Ti1 67.06(14) 5_656 4_556
O6 Sm1 Ti1 108.73(14) 6_666 4_556
O6 Sm1 Ti1 100.90(14) 2_655 4_556
O6 Sm1 Ti1 36.91(15) 4_556 4_556
O1 Sm1 Ti1 129.85(19) 2_655 .
O1 Sm1 Ti1 28.54(11) . .
O1 Sm1 Ti1 103.8(2) 3_665 .
O6 Sm1 Ti1 36.91(15) . .
O6 Sm1 Ti1 108.73(14) 3_665 .
O6 Sm1 Ti1 100.90(14) 5_656 .
O6 Sm1 Ti1 154.15(14) 6_666 .
O6 Sm1 Ti1 67.06(14) 2_655 .
O6 Sm1 Ti1 77.24(14) 4_556 .
Ti1 Sm1 Ti1 49.33(5) 4_556 .
O1 Sm1 Ti1 103.8(2) 2_655 3_665
O1 Sm1 Ti1 129.85(18) . 3_665
O1 Sm1 Ti1 28.54(11) 3_665 3_665
O6 Sm1 Ti1 67.07(14) . 3_665
O6 Sm1 Ti1 36.91(15) 3_665 3_665
O6 Sm1 Ti1 154.15(14) 5_656 3_665
O6 Sm1 Ti1 77.24(15) 6_666 3_665
O6 Sm1 Ti1 108.73(14) 2_655 3_665
O6 Sm1 Ti1 100.90(14) 4_556 3_665
Ti1 Sm1 Ti1 125.952(13) 4_556 3_665
Ti1 Sm1 Ti1 103.81(3) . 3_665
O21 Sm2 O21 120.000(10) 3_675 2_765
O21 Sm2 O21 119.999(4) 3_675 .
O21 Sm2 O21 120.001(3) 2_765 .
O21 Sm2 O25 66.0(2) 3_675 3_675
O21 Sm2 O25 136.16(15) 2_765 3_675
O21 Sm2 O25 71.6(2) . 3_675
O21 Sm2 O25 66.0(2) 3_675 6_677
O21 Sm2 O25 136.16(15) 2_765 6_677
O21 Sm2 O25 71.6(2) . 6_677
O25 Sm2 O25 87.4(3) 3_675 6_677
O21 Sm2 O25 71.6(2) 3_675 5_767
O21 Sm2 O25 66.0(2) 2_765 5_767
O21 Sm2 O25 136.16(15) . 5_767
O25 Sm2 O25 137.61(11) 3_675 5_767
O25 Sm2 O25 77.6(2) 6_677 5_767
O21 Sm2 O25 71.6(2) 3_675 2_765
O21 Sm2 O25 66.0(2) 2_765 2_765
O21 Sm2 O25 136.16(15) . 2_765
O25 Sm2 O25 77.6(2) 3_675 2_765
O25 Sm2 O25 137.61(11) 6_677 2_765
O25 Sm2 O25 87.4(3) 5_767 2_765
O21 Sm2 O25 136.16(15) 3_675 4_557
O21 Sm2 O25 71.6(2) 2_765 4_557
O21 Sm2 O25 66.0(2) . 4_557
O25 Sm2 O25 137.61(12) 3_675 4_557
O25 Sm2 O25 77.6(2) 6_677 4_557
O25 Sm2 O25 77.6(2) 5_767 4_557
O25 Sm2 O25 137.60(11) 2_765 4_557
O21 Sm2 O25 136.16(15) 3_675 .
O21 Sm2 O25 71.6(2) 2_765 .
O21 Sm2 O25 66.0(2) . .
O25 Sm2 O25 77.6(2) 3_675 .
O25 Sm2 O25 137.60(12) 6_677 .
O25 Sm2 O25 137.60(11) 5_767 .
O25 Sm2 O25 77.6(2) 2_765 .
O25 Sm2 O25 87.4(3) 4_557 .
O21 Sm2 Ti2 29.19(14) 3_675 6_677
O21 Sm2 Ti2 130.9(2) 2_765 6_677
O21 Sm2 Ti2 102.6(2) . 6_677
O25 Sm2 Ti2 77.43(15) 3_675 6_677
O25 Sm2 Ti2 37.44(16) 6_677 6_677
O25 Sm2 Ti2 66.51(16) 5_767 6_677
O25 Sm2 Ti2 100.24(16) 2_765 6_677
O25 Sm2 Ti2 109.16(15) 4_557 6_677
O25 Sm2 Ti2 154.75(16) . 6_677
O21 Sm2 Ti2 29.19(14) 3_675 3_675
O21 Sm2 Ti2 130.9(2) 2_765 3_675
O21 Sm2 Ti2 102.6(2) . 3_675
O25 Sm2 Ti2 37.44(16) 3_675 3_675
O25 Sm2 Ti2 77.43(15) 6_677 3_675
O25 Sm2 Ti2 100.24(16) 5_767 3_675
O25 Sm2 Ti2 66.51(16) 2_765 3_675
O25 Sm2 Ti2 154.75(16) 4_557 3_675
O25 Sm2 Ti2 109.16(15) . 3_675
Ti2 Sm2 Ti2 49.32(6) 6_677 3_675
O21 Sm2 Ti2 130.9(2) 3_675 .
O21 Sm2 Ti2 102.6(3) 2_765 .
O21 Sm2 Ti2 29.19(14) . .
O25 Sm2 Ti2 66.51(16) 3_675 .
O25 Sm2 Ti2 100.23(16) 6_677 .
O25 Sm2 Ti2 154.75(16) 5_767 .
O25 Sm2 Ti2 109.16(15) 2_765 .
O25 Sm2 Ti2 77.43(16) 4_557 .
O25 Sm2 Ti2 37.44(16) . .
Ti2 Sm2 Ti2 125.947(13) 6_677 .
Ti2 Sm2 Ti2 103.82(3) 3_675 .
O3 Ti1 O4 94.9(3) . .
O3 Ti1 O1 104.4(4) . .
O4 Ti1 O1 160.0(4) . .
O3 Ti1 O2 98.1(4) . .
O4 Ti1 O2 96.6(3) . .
O1 Ti1 O2 75.9(3) . .
O3 Ti1 O5 90.7(3) . .
O4 Ti1 O5 94.4(3) . .
O1 Ti1 O5 90.5(3) . .
O2 Ti1 O5 165.3(3) . .
O3 Ti1 O6 170.2(3) . .
O4 Ti1 O6 82.2(3) . .
O1 Ti1 O6 79.5(3) . .
O2 Ti1 O6 91.6(3) . .
O5 Ti1 O6 80.2(3) . .
O3 Ti1 Ti1 91.1(2) . 4_556
O4 Ti1 Ti1 138.3(2) . 4_556
O1 Ti1 Ti1 38.2(2) . 4_556
O2 Ti1 Ti1 41.7(2) . 4_556
O5 Ti1 Ti1 126.9(2) . 4_556
O6 Ti1 Ti1 97.27(16) . 4_556
O3 Ti1 Sm1 136.8(3) . .
O4 Ti1 Sm1 127.1(2) . .
O1 Ti1 Sm1 35.7(2) . .
O2 Ti1 Sm1 87.6(2) . .
O5 Ti1 Sm1 77.9(2) . .
O6 Ti1 Sm1 44.84(16) . .
Ti1 Ti1 Sm1 65.33(3) 4_556 .
O23 Ti2 O24 94.5(4) . .
O23 Ti2 O21 103.4(4) . .
O24 Ti2 O21 161.7(4) . .
O23 Ti2 O22 96.9(4) . .
O24 Ti2 O22 97.6(4) . .
O21 Ti2 O22 77.0(3) . .
O23 Ti2 O26 91.5(4) . .
O24 Ti2 O26 93.8(4) . .
O21 Ti2 O26 89.2(4) . .
O22 Ti2 O26 165.2(3) . .
O23 Ti2 O25 171.0(3) . .
O24 Ti2 O25 81.4(3) . .
O21 Ti2 O25 81.3(4) . .
O22 Ti2 O25 91.6(4) . .
O26 Ti2 O25 80.8(3) . .
O23 Ti2 Ti2 91.1(2) . 4_557
O24 Ti2 Ti2 139.2(2) . 4_557
O21 Ti2 Ti2 38.5(2) . 4_557
O22 Ti2 Ti2 41.6(2) . 4_557
O26 Ti2 Ti2 126.4(3) . 4_557
O25 Ti2 Ti2 97.18(17) . 4_557
O23 Ti2 Sm2 137.8(3) . .
O24 Ti2 Sm2 126.5(3) . .
O21 Ti2 Sm2 37.0(3) . .
O22 Ti2 Sm2 87.9(3) . .
O26 Ti2 Sm2 77.7(3) . .
O25 Ti2 Sm2 45.16(16) . .
Ti2 Ti2 Sm2 65.34(3) 4_557 .
Ti1 O1 Ti1 103.7(4) 4_556 .
Ti1 O1 Sm1 115.8(3) 4_556 .
Ti1 O1 Sm1 115.8(3) . .
C2 O2 Ti1 130.4(3) . .
C2 O2 Ti1 130.4(3) . 4_556
Ti1 O2 Ti1 96.7(4) . 4_556
C3' O3 Ti1 166.9(12) . .
C3 O3 Ti1 137.5(11) . .
C11 O4 Ti1 140.6(7) . .
C17 O5 Ti1 138.1(8) . .
C17 O6 Ti1 130.9(7) 3_665 .
C17 O6 Sm1 130.6(7) 3_665 .
Ti1 O6 Sm1 98.2(2) . .
Ti2 O21 Ti2 102.9(5) . 4_557
Ti2 O21 Sm2 113.9(4) . .
Ti2 O21 Sm2 113.9(4) 4_557 .
C22 O22 Ti2 130.3(3) . 4_557
C22 O22 Ti2 130.3(3) . .
Ti2 O22 Ti2 96.8(5) 4_557 .
C23' O23 Ti2 169.4(13) . .
C23 O23 Ti2 131.2(12) . .
C31 O24 Ti2 141.2(7) . .
C37 O25 Ti2 131.0(7) 2_765 .
C37 O25 Sm2 131.2(7) 2_765 .
Ti2 O25 Sm2 97.4(2) . .
C37 O26 Ti2 138.3(10) . .
C2A C2 O2 110.9(16) . .
C2A C2 C2B 135(2) . .
O2 C2 C2B 111.9(17) . .
C2A C2 H2A 94.5 . .
O2 C2 H2A 94.5 . .
C2B C2 H2A 94.5 . .
C2 C2A H2AA 109.5 . .
C2 C2A H2AB 109.5 . .
H2AA C2A H2AB 109.5 . .
C2 C2A H2AC 109.5 . .
H2AA C2A H2AC 109.5 . .
H2AB C2A H2AC 109.5 . .
C2 C2B H2BA 109.5 . .
C2 C2B H2BB 109.5 . .
H2BA C2B H2BB 109.5 . .
C2 C2B H2BC 109.5 . .
H2BA C2B H2BC 109.5 . .
H2BB C2B H2BC 109.5 . .
C3B C3 O3 109.5(17) . .
C3B C3 C3A 113(2) . .
O3 C3 C3A 111.1(18) . .
C3B C3 H3 107.8 . .
O3 C3 H3 107.8 . .
C3A C3 H3 107.8 . .
C3 C3A H3AA 109.5 . .
C3 C3A H3AB 109.5 . .
H3AA C3A H3AB 109.5 . .
C3 C3A H3AC 109.5 . .
H3AA C3A H3AC 109.5 . .
H3AB C3A H3AC 109.5 . .
C3 C3B H3BA 109.5 . .
C3 C3B H3BB 109.5 . .
H3BA C3B H3BB 109.5 . .
C3 C3B H3BC 109.5 . .
H3BA C3B H3BC 109.5 . .
H3BB C3B H3BC 109.5 . .
O3 C3' C3B' 120(2) . .
O3 C3' C3A' 111(2) . .
C3B' C3' C3A' 115(2) . .
O3 C3' H3A' 102.6 . .
C3B' C3' H3A' 102.6 . .
C3A' C3' H3A' 102.6 . .
C3' C3A' H3AD 109.5 . .
C3' C3A' H3AE 109.5 . .
H3AD C3A' H3AE 109.5 . .
C3' C3A' H3AF 109.5 . .
H3AD C3A' H3AF 109.5 . .
H3AE C3A' H3AF 109.5 . .
C3' C3B' H3BD 109.5 . .
C3' C3B' H3BE 109.5 . .
H3BD C3B' H3BE 109.5 . .
C3' C3B' H3BF 109.5 . .
H3BD C3B' H3BF 109.5 . .
H3BE C3B' H3BF 109.5 . .
O4 C11 C12 119.6(11) . .
O4 C11 C16 121.4(10) . .
C12 C11 C16 118.8(12) . .
C13 C12 C11 120.8(14) . .
C13 C12 H12A 119.6 . .
C11 C12 H12A 119.6 . .
C14 C13 C12 122.4(14) . .
C14 C13 H13A 118.8 . .
C12 C13 H13A 118.8 . .
C13 C14 C15 119.7(15) . .
C13 C14 H14A 120.1 . .
C15 C14 H14A 120.1 . .
C14 C15 C16 119.6(13) . .
C14 C15 H15A 120.2 . .
C16 C15 H15A 120.2 . .
C15 C16 C11 118.6(11) . .
C15 C16 C17 119.0(11) . 3_665
C11 C16 C17 122.4(10) . 3_665
O5 C17 O6 121.8(11) . 2_655
O5 C17 C16 116.1(10) . 2_655
O6 C17 C16 122.1(10) 2_655 2_655
C22B C22 O22 111(2) . .
C22B C22 C22A 134(3) . .
O22 C22 C22A 106(2) . .
C22B C22 H22' 99.5 . .
O22 C22 H22' 99.5 . .
C22A C22 H22' 99.5 . .
C22 C22A H22A 109.5 . .
C22 C22A H22B 109.5 . .
H22A C22A H22B 109.5 . .
C22 C22A H22C 109.5 . .
H22A C22A H22C 109.5 . .
H22B C22A H22C 109.5 . .
C22 C22B H22D 109.5 . .
C22 C22B H22E 109.5 . .
H22D C22B H22E 109.5 . .
C22 C22B H22F 109.5 . .
H22D C22B H22F 109.5 . .
H22E C22B H22F 109.5 . .
C23A C23 O23 111(2) . .
C23A C23 C23B 109(2) . .
O23 C23 C23B 109(2) . .
C23A C23 H23A 109.6 . .
O23 C23 H23A 109.6 . .
C23B C23 H23A 109.6 . .
C23 C23A H23B 109.5 . .
C23 C23A H23C 109.5 . .
H23B C23A H23C 109.5 . .
C23 C23A H23D 109.5 . .
H23B C23A H23D 109.5 . .
H23C C23A H23D 109.5 . .
C23 C23B H23E 109.5 . .
C23 C23B H23F 109.5 . .
H23E C23B H23F 109.5 . .
C23 C23B H23G 109.5 . .
H23E C23B H23G 109.5 . .
H23F C23B H23G 109.5 . .
C23C C23' O23 101(2) . .
C23C C23' C23D 112(2) . .
O23 C23' C23D 114(2) . .
C23C C23' H23H 110.0 . .
O23 C23' H23H 110.0 . .
C23D C23' H23H 110.0 . .
C23' C23C H23I 109.5 . .
C23' C23C H23J 109.5 . .
H23I C23C H23J 109.5 . .
C23' C23C H23K 109.5 . .
H23I C23C H23K 109.5 . .
H23J C23C H23K 109.5 . .
C23' C23D H23L 109.5 . .
C23' C23D H23M 109.5 . .
H23L C23D H23M 109.5 . .
C23' C23D H23N 109.5 . .
H23L C23D H23N 109.5 . .
H23M C23D H23N 109.5 . .
O24 C31 C32 119.7(12) . .
O24 C31 C36 121.4(10) . .
C32 C31 C36 118.9(12) . .
C33 C32 C31 121.0(14) . .
C33 C32 H32A 119.5 . .
C31 C32 H32A 119.5 . .
C34 C33 C32 121.2(13) . .
C34 C33 H33A 119.4 . .
C32 C33 H33A 119.4 . .
C33 C34 C35 118.6(14) . .
C33 C34 H34A 120.7 . .
C35 C34 H34A 120.7 . .
C36 C35 C34 121.1(14) . .
C36 C35 H35A 119.5 . .
C34 C35 H35A 119.5 . .
C35 C36 C31 119.1(11) . .
C35 C36 C37 118.3(11) . 2_765
C31 C36 C37 122.5(10) . 2_765
O26 C37 O25 121.9(12) . 3_675
O26 C37 C36 115.8(11) . 3_675
O25 C37 C36 122.4(10) 3_675 3_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 O1 2.317(9) 2_655
Sm1 O1 2.317(9) .
Sm1 O1 2.317(9) 3_665
Sm1 O6 2.550(6) .
Sm1 O6 2.550(6) 3_665
Sm1 O6 2.550(6) 5_656
Sm1 O6 2.550(6) 6_666
Sm1 O6 2.550(6) 2_655
Sm1 O6 2.550(6) 4_556
Sm1 Ti1 3.5784(16) 4_556
Sm1 Ti1 3.5785(16) .
Sm1 Ti1 3.5785(17) 3_665
Sm2 O21 2.355(10) 3_675
Sm2 O21 2.355(10) 2_765
Sm2 O21 2.355(10) .
Sm2 O25 2.562(6) 3_675
Sm2 O25 2.562(6) 6_677
Sm2 O25 2.562(6) 5_767
Sm2 O25 2.562(6) 2_765
Sm2 O25 2.562(6) 4_557
Sm2 O25 2.562(6) .
Sm2 Ti2 3.5834(18) 6_677
Sm2 Ti2 3.5834(18) 3_675
Sm2 Ti2 3.5834(18) .
Ti1 O3 1.772(7) .
Ti1 O4 1.883(7) .
Ti1 O1 1.899(5) .
Ti1 O2 1.999(6) .
Ti1 O5 2.013(7) .
Ti1 O6 2.171(7) .
Ti1 Ti1 2.987(3) 4_556
Ti2 O23 1.780(8) .
Ti2 O24 1.872(8) .
Ti2 O21 1.911(6) .
Ti2 O22 1.999(8) .
Ti2 O26 2.020(9) .
Ti2 O25 2.197(8) .
Ti2 Ti2 2.990(3) 4_557
O2 C2 1.470(18) .
O3 C3' 1.38(2) .
O3 C3 1.44(2) .
O4 C11 1.339(13) .
O5 C17 1.267(15) .
O6 C17 1.293(13) 3_665
O22 C22 1.45(3) .
O23 C23' 1.43(2) .
O23 C23 1.47(2) .
O24 C31 1.327(14) .
O25 C37 1.267(14) 2_765
O26 C37 1.258(12) .
C2 C2A 1.45(3) .
C2 C2B 1.56(4) .
C2 H2A 1.0000 .
C2A H2AA 0.9800 .
C2A H2AB 0.9800 .
C2A H2AC 0.9800 .
C2B H2BA 0.9800 .
C2B H2BB 0.9800 .
C2B H2BC 0.9800 .
C3 C3B 1.42(2) .
C3 C3A 1.45(2) .
C3 H3 1.0000 .
C3A H3AA 0.9800 .
C3A H3AB 0.9800 .
C3A H3AC 0.9800 .
C3B H3BA 0.9800 .
C3B H3BB 0.9800 .
C3B H3BC 0.9800 .
C3' C3B' 1.39(2) .
C3' C3A' 1.45(2) .
C3' H3A' 1.0000 .
C3A' H3AD 0.9800 .
C3A' H3AE 0.9800 .
C3A' H3AF 0.9800 .
C3B' H3BD 0.9800 .
C3B' H3BE 0.9800 .
C3B' H3BF 0.9800 .
C11 C12 1.379(15) .
C11 C16 1.407(17) .
C12 C13 1.35(2) .
C12 H12A 0.9500 .
C13 C14 1.33(2) .
C13 H13A 0.9500 .
C14 C15 1.398(19) .
C14 H14A 0.9500 .
C15 C16 1.403(17) .
C15 H15A 0.9500 .
C16 C17 1.488(16) 3_665
C22 C22B 1.44(4) .
C22 C22A 1.52(5) .
C22 H22' 1.0000 .
C22A H22A 0.9800 .
C22A H22B 0.9800 .
C22A H22C 0.9800 .
C22B H22D 0.9800 .
C22B H22E 0.9800 .
C22B H22F 0.9800 .
C23 C23A 1.46(3) .
C23 C23B 1.47(3) .
C23 H23A 1.0000 .
C23A H23B 0.9800 .
C23A H23C 0.9800 .
C23A H23D 0.9800 .
C23B H23E 0.9800 .
C23B H23F 0.9800 .
C23B H23G 0.9800 .
C23' C23C 1.35(3) .
C23' C23D 1.45(3) .
C23' H23H 1.0000 .
C23C H23I 0.9800 .
C23C H23J 0.9800 .
C23C H23K 0.9800 .
C23D H23L 0.9800 .
C23D H23M 0.9800 .
C23D H23N 0.9800 .
C31 C32 1.390(16) .
C31 C36 1.412(17) .
C32 C33 1.38(2) .
C32 H32A 0.9500 .
C33 C34 1.37(2) .
C33 H33A 0.9500 .
C34 C35 1.408(18) .
C34 H34A 0.9500 .
C35 C36 1.393(16) .
C35 H35A 0.9500 .
C36 C37 1.467(16) 2_765
