A simple one-pot route to stable formamidinatoiodidolanthanoid(III) complexes from lanthanoid metals.
Guo, Zhifang; Blair, Victoria L.; Deacon, Glen B.; Junk, Peter C.; Chemical communications (Cambridge, England) 57 (2021) 11513–11516; doi:10.1039/d1cc04080d

data_7129080
_publ_section_title
;
 A simple one-pot route to stable formamidinatoiodidolanthanoid(III)
 complexes from lanthanoid metals.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11513
_journal_page_last               11516
_journal_paper_doi               10.1039/d1cc04080d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C37 H59 I2 Lu N2 O3, 2(C4 H8 O)'
_chemical_formula_sum            'C45 H75 I2 Lu N2 O5'
_chemical_formula_weight         1152.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2021-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                99.391(2)
_cell_angle_beta                 106.182(3)
_cell_angle_gamma                97.937(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6323(3)
_cell_length_b                   13.4896(3)
_cell_length_c                   16.2376(5)
_cell_measurement_reflns_used    14797
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      30.0900
_cell_measurement_theta_min      2.5110
_cell_volume                     2368.45(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -17.00  39.00   0.50    1.77    --    4.01-102.00-107.00  112
  2  \w    -17.00  30.00   0.50    1.77    --   -5.11-102.00-107.00   94
  3  \w     -9.00  77.00   0.50    1.77    --    4.01  38.00   0.00  172
  4  \w    -26.00  38.00   0.50    1.77    --    4.01 -99.00 -60.00  128
  5  \w    -69.00  27.00   0.50    1.77    --    4.01 -77.00-180.00  192
  6  \w    -26.00  38.00   0.50    1.77    --    4.01 -99.00  90.00  128
  7  \w     -9.00  77.00   0.50    1.77    --    4.01  38.00 -90.00  172
  8  \w    -26.00  28.00   0.50    1.77    --   -5.11 -99.00-150.00  108
  9  \w    -77.00 -15.00   0.50    1.77    --   -5.11 -57.00 -90.00  124
 10  \w    -24.00  20.00   0.50    1.77    --   -5.11 -99.00  30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0600188000
_diffrn_orient_matrix_UB_12      0.0019910000
_diffrn_orient_matrix_UB_13      -0.0249139000
_diffrn_orient_matrix_UB_21      -0.0202555000
_diffrn_orient_matrix_UB_22      -0.0040815000
_diffrn_orient_matrix_UB_23      0.0368857000
_diffrn_orient_matrix_UB_31      0.0132615000
_diffrn_orient_matrix_UB_32      0.0541345000
_diffrn_orient_matrix_UB_33      0.0135988000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42943
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.526
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.938
_refine_diff_density_min         -2.575
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8330
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0492
_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/[\s^2^(Fo^2^)+(0.0879P)^2^+1.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6900
_reflns_number_total             8330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_database_code               7129080
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         LuICHNO
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.547
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Restrained distances
 I2-Lu1 \\sim Lu1-I2A
 with sigma of 0.02
 I1A-Lu1 \\sim Lu1-I1
 with sigma of 0.02
2. Rigid bond restraints
 I1A, I1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 I2A, I2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
I1A \\sim I1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
I2A \\sim I2: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Others
 Sof(I1A)=1-FVAR(1)
 Sof(I1)=FVAR(1)
 Sof(I2)=1-FVAR(2)
 Sof(I2A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C23(H23), C10(H10), C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C30(H30A,H30B), C29(H29A,H29B), C36(H36A,H36B), C31(H31A,
 H31B), C26(H26A,H26B), C34(H34A,H34B), C35(H35A,H35B), C43(H43A,H43B),
 C45(H45A,H45B), C33(H33A,H33B), C42(H42A,H42B), C32(H32A,H32B), C39(H39A,H39B),
  C44(H44A,H44B), C27(H27A,H27B), C28(H28A,H28B), C40(H40A,H40B), C38(H38A,
 H38B), C41(H41A,H41B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C21(H21), C7(H7), C19(H19), C20(H20)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C3(H3A,H3B,H3C), C17(H17A,H17B,H17C), C1(H1A,H1B,H1C),
 C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              44849
_shelx_hkl_checksum              12554
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.227
_oxdiff_exptl_absorpt_empirical_full_min 0.237