#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:09:35 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224430 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/98/7049881.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_7049881
loop_
_publ_author_name
'Gompa, Thaige P.'
'Rice, Natalie T.'
'Russo, Dominic R.'
'Aguirre Quintana, Luis M.'
'Yik, Brandon J.'
'Bacsa, John'
'La Pierre, Henry S.'
_publ_section_title
;
 Diethyl ether adducts of trivalent lanthanide iodides.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8030
_journal_page_last               8033
_journal_paper_doi               10.1039/c9dt00775j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H40 I2 O5 Tb, C8 H16 I4 O2 Tb'
_chemical_formula_sum            'C28 H56 I6 O7 Tb2'
_chemical_formula_weight         1583.96
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     dual
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.06.21 svn.r3421 for OlexSys, GUI svn.r5355)
;
_audit_update_record
;
2019-02-19 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.442(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.742(3)
_cell_length_b                   12.016(3)
_cell_length_c                   28.632(6)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.823
_cell_measurement_theta_min      2.342
_cell_volume                     4336.3(17)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            35946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.139
_diffrn_reflns_theta_min         2.342
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.542
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.3986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1196 before and 0.0856 after correction. The Ratio of minimum to maximum transmission is 0.5350. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             2912
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0128P)²+18.0819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6594
_reflns_number_total             8278
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00775j2.cif
_cod_data_source_block           tbi3thf3
_cod_depositor_comments
'Adding full bibliography for 7049875--7049882.cif.'
_cod_original_cell_volume        4336.3(16)
_cod_database_code               7049881
_shelx_shelxl_version_number     2014/7
_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_max   0.494
_shelx_estimated_absorpt_t_min   0.339
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Rigid body (RIGU) restrains
 O4, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C8(H8A,H8B), C13(H13A,H13B), C2(H2A,H2B), C3(H3A,
 H3B), C14(H14A,H14B), C1(H1A,H1B), C9(H9A,H9B), C4(H4A,H4B), C7(H7A,H7B),
 C11(H11A,H11B), C6(H6A,H6B), C10(H10A,H10B)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id TbI3THF3
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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'
'-x, -y, -z'
'x, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Tb2 Tb 0.5000 0.49933(2) 0.2500 0.00873(4) Uani 1 2 d S T P
Tb1 Tb 0.0000 0.5000 0.5000 0.01092(4) Uani 1 2 d S T P
I2 I 0.08754(2) 0.59783(2) 0.59526(2) 0.01723(5) Uani 1 1 d . . .
I1 I 0.02972(2) 0.26697(2) 0.53796(2) 0.01776(5) Uani 1 1 d . . .
I3 I 0.28881(2) 0.49786(2) 0.28318(2) 0.01720(5) Uani 1 1 d . . .
O3 O 0.5000 0.6985(3) 0.2500 0.0137(6) Uani 1 2 d S T P
O2 O 0.45204(19) 0.33912(19) 0.20217(8) 0.0139(4) Uani 1 1 d . . .
O1 O 0.1728(2) 0.5042(2) 0.48332(9) 0.0162(5) Uani 1 1 d . . .
O4 O 0.5831(2) 0.5622(2) 0.32654(8) 0.0154(5) Uani 1 1 d . U .
C5 C 0.5227(3) 0.2517(3) 0.18893(13) 0.0182(7) Uani 1 1 d . . .
H5A H 0.5699 0.2238 0.2170 0.022 Uiso 1 1 calc R . .
H5B H 0.5668 0.2802 0.1658 0.022 Uiso 1 1 calc R . .
C12 C 0.6792(3) 0.6311(3) 0.33495(13) 0.0203(7) Uani 1 1 d . U .
H12A H 0.6794 0.6870 0.3096 0.024 Uiso 1 1 calc R . .
H12B H 0.7437 0.5845 0.3364 0.024 Uiso 1 1 calc R . .
C8 C 0.3422(3) 0.3135(3) 0.18141(12) 0.0162(6) Uani 1 1 d . . .
H8A H 0.3064 0.3805 0.1665 0.019 Uiso 1 1 calc R . .
H8B H 0.3013 0.2854 0.2058 0.019 Uiso 1 1 calc R . .
C13 C 0.4462(3) 0.7690(3) 0.28107(12) 0.0156(6) Uani 1 1 d . . .
H13A H 0.4621 0.7435 0.3142 0.019 Uiso 1 1 calc R . .
H13B H 0.3684 0.7676 0.2712 0.019 Uiso 1 1 calc R . .
C2 C 0.2760(3) 0.4699(3) 0.42367(13) 0.0201(7) Uani 1 1 d . . .
H2A H 0.2279 0.5005 0.3964 0.024 Uiso 1 1 calc R . .
H2B H 0.3276 0.4189 0.4122 0.024 Uiso 1 1 calc R . .
C3 C 0.3318(3) 0.5625(3) 0.45454(15) 0.0237(8) Uani 1 1 d . . .
H3A H 0.3512 0.6251 0.4350 0.028 Uiso 1 1 calc R . .
H3B H 0.3966 0.5343 0.4743 0.028 Uiso 1 1 calc R . .
C14 C 0.4899(3) 0.8845(3) 0.27572(12) 0.0176(7) Uani 1 1 d . . .
H14A H 0.5564 0.8966 0.2977 0.021 Uiso 1 1 calc R . .
H14B H 0.4377 0.9424 0.2812 0.021 Uiso 1 1 calc R . .
C1 C 0.2154(3) 0.4132(3) 0.45796(13) 0.0175(7) Uani 1 1 d . . .
H1A H 0.1574 0.3670 0.4412 0.021 Uiso 1 1 calc R . .
H1B H 0.2627 0.3653 0.4799 0.021 Uiso 1 1 calc R . .
C9 C 0.5449(4) 0.5423(4) 0.37201(12) 0.0246(8) Uani 1 1 d . U .
H9A H 0.5397 0.4615 0.3781 0.030 Uiso 1 1 calc R . .
H9B H 0.4742 0.5765 0.3721 0.030 Uiso 1 1 calc R . .
C4 C 0.2482(3) 0.5984(3) 0.48509(13) 0.0182(7) Uani 1 1 d . . .
H4A H 0.2816 0.6127 0.5180 0.022 Uiso 1 1 calc R . .
H4B H 0.2114 0.6668 0.4723 0.022 Uiso 1 1 calc R . .
C7 C 0.3521(3) 0.2249(3) 0.14485(13) 0.0198(7) Uani 1 1 d . . .
H7A H 0.3634 0.2582 0.1143 0.024 Uiso 1 1 calc R . .
H7B H 0.2885 0.1767 0.1398 0.024 Uiso 1 1 calc R . .
C11 C 0.6745(4) 0.6865(4) 0.38151(15) 0.0314(9) Uani 1 1 d . U .
H11A H 0.6288 0.7534 0.3777 0.038 Uiso 1 1 calc R . .
H11B H 0.7462 0.7077 0.3972 0.038 Uiso 1 1 calc R . .
C6 C 0.4491(3) 0.1609(3) 0.16728(14) 0.0220(8) Uani 1 1 d . . .
H6A H 0.4312 0.1088 0.1917 0.026 Uiso 1 1 calc R . .
H6B H 0.4813 0.1186 0.1433 0.026 Uiso 1 1 calc R . .
C10 C 0.6268(4) 0.5964(4) 0.40893(15) 0.0336(9) Uani 1 1 d . U .
H10A H 0.5931 0.6287 0.4349 0.040 Uiso 1 1 calc R . .
H10B H 0.6814 0.5420 0.4223 0.040 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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Tb Tb -0.1723 4.1537 '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
I3 Tb2 I3 179.322(12) 2_655 .
O3 Tb2 I3 90.340(6) . .
O3 Tb2 I3 90.339(6) . 2_655
O3 Tb2 O4 71.75(6) . 2_655
O3 Tb2 O4 71.75(6) . .
O2 Tb2 I3 88.83(6) 2_655 .
O2 Tb2 I3 90.63(6) 2_655 2_655
O2 Tb2 I3 90.63(6) . .
O2 Tb2 I3 88.83(6) . 2_655
O2 Tb2 O3 143.68(6) 2_655 .
O2 Tb2 O3 143.68(6) . .
O2 Tb2 O2 72.64(11) 2_655 .
O2 Tb2 O4 71.95(8) . 2_655
O2 Tb2 O4 144.54(8) . .
O2 Tb2 O4 144.54(8) 2_655 2_655
O2 Tb2 O4 71.95(8) 2_655 .
O4 Tb2 I3 90.50(6) 2_655 2_655
O4 Tb2 I3 89.71(6) . 2_655
O4 Tb2 I3 90.50(6) . .
O4 Tb2 I3 89.71(6) 2_655 .
O4 Tb2 O4 143.50(12) 2_655 .
I2 Tb1 I2 180.0 . 5_566
I1 Tb1 I2 88.523(13) 5_566 .
I1 Tb1 I2 91.476(13) 5_566 5_566
I1 Tb1 I2 91.478(13) . .
I1 Tb1 I2 88.522(13) . 5_566
I1 Tb1 I1 180.0 . 5_566
O1 Tb1 I2 93.34(6) . 5_566
O1 Tb1 I2 86.66(6) . .
O1 Tb1 I2 93.34(6) 5_566 .
O1 Tb1 I2 86.66(6) 5_566 5_566
O1 Tb1 I1 88.76(6) 5_566 .
O1 Tb1 I1 91.24(6) . .
O1 Tb1 I1 88.75(6) . 5_566
O1 Tb1 I1 91.25(6) 5_566 5_566
O1 Tb1 O1 180.00(11) 5_566 .
C13 O3 Tb2 125.21(17) 2_655 .
C13 O3 Tb2 125.21(17) . .
C13 O3 C13 109.6(3) 2_655 .
C5 O2 Tb2 127.5(2) . .
C5 O2 C8 109.2(2) . .
C8 O2 Tb2 123.28(18) . .
C1 O1 Tb1 121.3(2) . .
C1 O1 C4 107.6(3) . .
C4 O1 Tb1 129.8(2) . .
C12 O4 Tb2 124.7(2) . .
C12 O4 C9 108.8(3) . .
C9 O4 Tb2 126.4(2) . .
O2 C5 H5A 110.8 . .
O2 C5 H5B 110.8 . .
O2 C5 C6 104.8(3) . .
H5A C5 H5B 108.9 . .
C6 C5 H5A 110.8 . .
C6 C5 H5B 110.8 . .
O4 C12 H12A 110.8 . .
O4 C12 H12B 110.8 . .
O4 C12 C11 104.8(3) . .
H12A C12 H12B 108.9 . .
C11 C12 H12A 110.8 . .
C11 C12 H12B 110.8 . .
O2 C8 H8A 110.8 . .
O2 C8 H8B 110.8 . .
O2 C8 C7 104.9(3) . .
H8A C8 H8B 108.8 . .
C7 C8 H8A 110.8 . .
C7 C8 H8B 110.8 . .
O3 C13 H13A 110.8 . .
O3 C13 H13B 110.8 . .
O3 C13 C14 104.9(3) . .
H13A C13 H13B 108.8 . .
C14 C13 H13A 110.8 . .
C14 C13 H13B 110.8 . .
H2A C2 H2B 109.4 . .
C3 C2 H2A 111.6 . .
C3 C2 H2B 111.6 . .
C1 C2 H2A 111.6 . .
C1 C2 H2B 111.6 . .
C1 C2 C3 101.1(3) . .
C2 C3 H3A 111.1 . .
C2 C3 H3B 111.1 . .
C2 C3 C4 103.3(3) . .
H3A C3 H3B 109.1 . .
C4 C3 H3A 111.1 . .
C4 C3 H3B 111.1 . .
C13 C14 C14 102.3(2) . 2_655
C13 C14 H14A 111.3 . .
C13 C14 H14B 111.3 . .
C14 C14 H14A 111.3 2_655 .
C14 C14 H14B 111.3 2_655 .
H14A C14 H14B 109.2 . .
O1 C1 C2 104.5(3) . .
O1 C1 H1A 110.9 . .
O1 C1 H1B 110.9 . .
C2 C1 H1A 110.9 . .
C2 C1 H1B 110.9 . .
H1A C1 H1B 108.9 . .
O4 C9 H9A 110.7 . .
O4 C9 H9B 110.7 . .
O4 C9 C10 105.2(3) . .
H9A C9 H9B 108.8 . .
C10 C9 H9A 110.7 . .
C10 C9 H9B 110.7 . .
O1 C4 C3 105.5(3) . .
O1 C4 H4A 110.6 . .
O1 C4 H4B 110.6 . .
C3 C4 H4A 110.6 . .
C3 C4 H4B 110.6 . .
H4A C4 H4B 108.8 . .
C8 C7 H7A 111.4 . .
C8 C7 H7B 111.4 . .
C8 C7 C6 102.1(3) . .
H7A C7 H7B 109.2 . .
C6 C7 H7A 111.4 . .
C6 C7 H7B 111.4 . .
C12 C11 H11A 111.3 . .
C12 C11 H11B 111.3 . .
C12 C11 C10 102.4(3) . .
H11A C11 H11B 109.2 . .
C10 C11 H11A 111.3 . .
C10 C11 H11B 111.3 . .
C5 C6 C7 103.0(3) . .
C5 C6 H6A 111.2 . .
C5 C6 H6B 111.2 . .
C7 C6 H6A 111.2 . .
C7 C6 H6B 111.2 . .
H6A C6 H6B 109.1 . .
C9 C10 H10A 111.1 . .
C9 C10 H10B 111.1 . .
C11 C10 C9 103.4(3) . .
C11 C10 H10A 111.1 . .
C11 C10 H10B 111.1 . .
H10A C10 H10B 109.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb2 I3 2.9824(6) 2_655
Tb2 I3 2.9824(6) .
Tb2 O3 2.393(3) .
Tb2 O2 2.389(2) 2_655
Tb2 O2 2.389(2) .
Tb2 O4 2.411(2) 2_655
Tb2 O4 2.411(2) .
Tb1 I2 3.0284(5) .
Tb1 I2 3.0285(5) 5_566
Tb1 I1 3.0074(6) 5_566
Tb1 I1 3.0073(6) .
Tb1 O1 2.321(2) .
Tb1 O1 2.321(2) 5_566
O3 C13 1.469(4) .
O3 C13 1.469(4) 2_655
O2 C5 1.469(4) .
O2 C8 1.470(4) .
O1 C1 1.460(4) .
O1 C4 1.480(4) .
O4 C12 1.468(4) .
O4 C9 1.475(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C5 C6 1.511(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C12 C11 1.499(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C8 C7 1.511(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C13 C14 1.512(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.530(6) .
C2 C1 1.499(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C3 C4 1.536(5) .
C14 C14 1.532(7) 2_655
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C9 C10 1.519(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C7 C6 1.516(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C11 C10 1.516(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
