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_7049880
_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_absolute_configuration ad
_chemical_formula_moiety         'C12 H30 I3 Nd O3'
_chemical_formula_sum            'C12 H30 I3 Nd O3'
_chemical_formula_weight         747.30
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-08
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3167(5)
_cell_length_b                   16.1003(9)
_cell_length_c                   13.6533(9)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.281
_cell_measurement_theta_min      2.94
_cell_volume                     2267.8(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.992
_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  0.0356
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39636
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.375
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.1738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1199 before and 0.0672 after correction. The Ratio of minimum to maximum transmission is 0.2326. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.233
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details
;
 Flack x determined using 2249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+20.0269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                4964
_reflns_number_total             5126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00775j2.cif
_cod_data_source_block           bjy-01-081_l
_cod_depositor_comments
'Adding full bibliography for 7049875--7049882.cif.'
_cod_database_code               7049880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.087
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.74(4)
 0.26(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C9, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C11(H11A,H11B), C7(H7A,H7B), C3(H3A,H3B), C1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              53921
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_original_sample_id BJY-01-081
_olex2_submission_special_instructions 'No special instructions were received'