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_7049878
_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         'C12 H30 I3 O3 Tm'
_chemical_formula_sum            'C12 H30 I3 O3 Tm'
_chemical_formula_weight         771.99
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-02-18 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                65.386(7)
_cell_angle_beta                 87.540(7)
_cell_angle_gamma                87.044(7)
_cell_formula_units_Z            8
_cell_length_a                   13.695(2)
_cell_length_b                   17.532(3)
_cell_length_c                   20.912(4)
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.465
_cell_volume                     4557.4(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88713
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.143
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.959
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1327 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.5998. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_description       prism
_exptl_crystal_F_000             2832
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.396
_refine_diff_density_min         -4.347
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         17277
_refine_ls_number_restraints     1113
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+148.1951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15297
_reflns_number_total             17277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00775j2.cif
_cod_data_source_block           tmi3c4h8o
_cod_depositor_comments
'Adding full bibliography for 7049875--7049882.cif.'
_cod_original_cell_volume        4557.7(15)
_cod_database_code               7049878
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.210
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10_2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C2_4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Tm1_5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C2_4) = Uanis(C2_5)
Uanis(C1_4) = Uanis(C1_5)
Uanis(O1_4) = Uanis(O1_5)
Uanis(C4_4) = Uanis(C4_5)
Uanis(C10_4) = Uanis(C10_5)
Uanis(O3_4) = Uanis(O3_5)
Uanis(C8_4) = Uanis(C8_5)
Uanis(C12_4) = Uanis(C12_5)
Uanis(C11_4) = Uanis(C11_5)
Uanis(C6_4) = Uanis(C6_5)
Uanis(C9_4) = Uanis(C9_5)
Uanis(I3_4) = Uanis(I3_5)
Uanis(I2_4) = Uanis(I2_5)
Uanis(Tm1_5) = Uanis(Tm1_4)
Uanis(C3_5) = Uanis(C3_4)
Uanis(C5_5) = Uanis(C5_4)
Uanis(I1_4) = Uanis(I1_5)
3. Rigid body (RIGU) restrains
 Tm1_2, I1_2, I2_2, I3_2, O1_2, O2_2, O3_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2,
  C7_2, C8_2, C9_2, C10_2, C11_2, C12_2
 Tm1_3, I1_3, I2_3, I3_3, O1_3, O2_3, O3_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3,
  C7_3, C8_3, C9_3, C10_3, C11_3, C12_3
 Tm1_1, I1_1, I2_1, I3_1, O1_1, O2_1, O3_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1,
  C7_1, C8_1, C9_1, C10_1, C11_1, C12_1
 Tm1_4, I1_4, I2_4, I3_4, O1_4, O2_4, O3_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4,
  C7_4, C8_4, C9_4, C10_4, C11_4, C12_4
 Tm1_5, I1_5, I2_5, I3_5, O1_5, O2_5, O3_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5,
  C7_5, C8_5, C9_5, C10_5, C11_5, C12_5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Tm1_3, I1_3, I2_3, I3_3, O1_3, O2_3, O3_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3,
C7_3, C8_3, C9_3, C10_3, C11_3, C12_3}
{Tm1_1, I1_1, I2_1, I3_1, O1_1, O2_1, O3_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1,
C7_1, C8_1, C9_1, C10_1, C11_1, C12_1}
{Tm1_4, I1_4, I2_4, I3_4, O1_4, O2_4, O3_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4,
C7_4, C8_4, C9_4, C10_4, C11_4, C12_4}
{Tm1_5, I1_5, I2_5, I3_5, O1_5, O2_5, O3_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5,
C7_5, C8_5, C9_5, C10_5, C11_5, C12_5}
as
{Tm1_2, I1_2, I2_2, I3_2, O1_2, O2_2, O3_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2,
C7_2, C8_2, C9_2, C10_2, C11_2, C12_2} sigma for 1-2: 0.002 1-3: 0.04
5. Others
 Sof(Tm1)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(1)
 Sof(Tm1)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B),
 C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,
 H9B), C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B),
 C9(H9A,H9B), C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,
 H7B), C9(H9A,H9B), C11(H11A,H11B)
6.b Idealised Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C2(H2A,
 H2B,H2C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C),
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C6(H6A,
 H6B,H6C)
;
_shelx_res_checksum              71387
_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 TmI3C4H8O
_olex2_submission_special_instructions 'No special instructions were received'