Diethyl ether adducts of trivalent lanthanide iodides.
Gompa, Thaige P.; Rice, Natalie T.; Russo, Dominic R.; Aguirre Quintana, Luis M.; Yik, Brandon J.; Bacsa, John; La Pierre, Henry S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8030–8033; doi:10.1039/c9dt00775j

data_7049881
_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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0128P)^2^+18.0819P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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'