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_7129081
_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 N2 Nd O3, C4 H8 O'
_chemical_formula_sum            'C41 H67 I2 N2 Nd O4'
_chemical_formula_weight         1050.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6958(3)
_cell_length_b                   18.9803(3)
_cell_length_c                   24.0171(5)
_cell_measurement_reflns_used    7909
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     8978.4(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53865
_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         2.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57640
_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            purple
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0243P)^2^+30.6125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6474
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_database_code               7129081
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.627
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C41 = O4-C38
 1.44 with sigma of 0.02
 C41-C40 = C39-C38
 1.53 with sigma of 0.02
 C40-C39
 1.54 with sigma of 0.02
 O5-C45 = O5-C42
 1.44 with sigma of 0.02
 C45-C44 = C43-C42
 1.53 with sigma of 0.02
 C44-C43
 1.54 with sigma of 0.02
 O4-C40 = O4-C39 = C41-C39 = C40-C38
 2.38 with sigma of 0.04
 O5-C44 = O5-C43 = C45-C43 = C44-C42
 2.38 with sigma of 0.04
 O5-C44 \\sim O5-C43
 with sigma of 0.04
 C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 O5-C45 \\sim O5-C42
 with sigma of 0.02
 C44-C42 \\sim C45-C43
 with sigma of 0.04
 C41-C40 \\sim C40-C39 \\sim C39-C38
 with sigma of 0.02
 O4-C41 \\sim O4-C38
 with sigma of 0.02
 O4-C40 \\sim O4-C39
 with sigma of 0.04
 C40-C38 \\sim C41-C39
 with sigma of 0.04
3. Rigid bond restraints
 C42, C43, C44, C45, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O4 \\sim C41 \\sim C40 \\sim C39 \\sim C38: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O5 \\sim C45 \\sim C44 \\sim C43 \\sim C42: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C42 \\sim C43 \\sim C44 \\sim C45 \\sim C38 \\sim C39 \\sim C40 \\sim C41:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
5. Rigid body (RIGU) restrains
 O4, C41, C40, C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C45, C44, C43, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) H35A(0.5) H35B(0.5)
 H35C(0.5) H35D(0.5) C36(0.5) H36A(0.5) H36B(0.5) C36A(0.5) H36C(0.5) H36D(0.5)
 O4(0.5) C41(0.5) H41A(0.5) H41B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C39(0.5)
 H39A(0.5) H39B(0.5) C38(0.5) H38A(0.5) H38B(0.5) O5(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C42(0.5)
 H42A(0.5) H42B(0.5)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C23(H23), C16(H16), C3(H3)
7.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C37(H37A,H37B), C37(H37C,H37D), C29(H29A,H29B), C27(H27A,
 H27B), C28(H28A,H28B), C30(H30A,H30B), C34(H34A,H34B), C35(H35A,H35B),
 C35(H35C,H35D), C32(H32A,H32B), C33(H33A,H33B), C36(H36A,H36B), C31(H31A,H31B),
  C36A(H36C,H36D), C41(H41A,H41B), C40(H40A,H40B), C39(H39A,H39B), C38(H38A,
 H38B), C45(H45A,H45B), C44(H44A,H44B), C43(H43A,H43B), C42(H42A,H42B)
7.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C6(H6), C19(H19), C21(H21), C5(H5), C20(H20), C7(H7)
7.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C12(H12A,H12B,H12C), C24(H24A,H24B,
 H24C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C25(H25A,H25B,H25C), C1(H1A,H1B,
 H1C)
;
_shelx_res_checksum              12284
_shelx_hkl_checksum              87488
_olex2_submission_special_instructions 'No special instructions were received'