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_7129083
_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 Gd I2 N2 O3, C4 H8 O'
_chemical_formula_sum            'C41 H67 Gd I2 N2 O4'
_chemical_formula_weight         1063.01
_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
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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                   18.831(4)
_cell_length_b                   19.561(4)
_cell_length_c                   24.134(5)
_cell_measurement_reflns_used    7576
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     8890(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            93420
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.688
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             4232
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         7576
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+208.8637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6858
_reflns_number_total             7576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_database_code               7129083
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Restrained distances
 C38-C39 = C40-C41
 1.53 with sigma of 0.02
 C45-C44 = C43-C42
 1.53 with sigma of 0.02
 O4-C38 = O4-C41
 1.44 with sigma of 0.02
 C39-C40
 1.54 with sigma of 0.02
 O5-C45 = O5-C42
 1.44 with sigma of 0.02
 C44-C43
 1.54 with sigma of 0.02
 O5-C44 = O5-C43 = C45-C43 = C44-C42
 2.38 with sigma of 0.04
 O4-C39 = O4-C40 = C38-C40 = C39-C41
 2.38 with sigma of 0.04
 C26-C27 \\sim C26A-C27 \\sim C28A-C29A \\sim C28A-C27 \\sim C28-C27 \\sim
C29-C28
 with sigma of 0.02
 O2-C33 \\sim O2-C30 \\sim O2-C33A \\sim O2-C30A
 with sigma of 0.02
 C32A-C33A \\sim C33-C32 \\sim C31A-C30A \\sim C31A-C32A \\sim C32-C31 \\sim
C30-C31
 with sigma of 0.02
 O3-C34A \\sim O3-C34 \\sim O3-C37 \\sim O3-C37A
 with sigma of 0.02
 C35-C34 \\sim C35-C36 \\sim C35A-C34A \\sim C37-C36 \\sim C36A-C35A \\sim
C37A-C36A
 with sigma of 0.02
 C38-C39 \\sim C39-C40 \\sim C40-C41
 with sigma of 0.02
 O4-C39 \\sim O4-C40
 with sigma of 0.04
 O4-C38 \\sim O4-C41
 with sigma of 0.02
 C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.02
 O5-C45 \\sim O5-C42
 with sigma of 0.02
 C39-C41 \\sim C38-C40
 with sigma of 0.04
 O5-C44 \\sim O5-C43
 with sigma of 0.04
 C44-C42 \\sim C45-C43
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C22A \\sim C20A \\sim C21A \\sim C22 \\sim C20 \\sim C21: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.01 within 2A
C26 \\sim C26A \\sim C27 \\sim C28A \\sim C28 \\sim C29 \\sim C29A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C33A \\sim C32A \\sim C33 \\sim C32 \\sim C30A \\sim C30 \\sim C31A \\sim C31:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C34A \\sim C35A \\sim C36A \\sim C37A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
O4 \\sim C38 \\sim C39 \\sim C40 \\sim C41: 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
3. Rigid body (RIGU) restrains
 C22, C20, C21, C21A, C20A, C22A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C26, C26A, C29, C28, C29A, C28A, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33A, C32A, C33, C32, C31A, C30A, C30, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C34A, C35, C36, C35A, C37, C37A, C36A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5, C45, C44, C43, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(I2)=1-FVAR(1)
 Sof(I3)=FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C21A)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(2)
 Sof(C22)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=FVAR(2)
 Sof(H27A)=Sof(H27B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(C28A)=Sof(H28A)=
 Sof(H28B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=1-FVAR(3)
 Sof(H27C)=Sof(H27D)=Sof(C29)=Sof(H29C)=Sof(H29D)=Sof(C28)=Sof(H28C)=Sof(H28D)=
 Sof(C26)=Sof(H26C)=Sof(H26D)=FVAR(3)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=1-FVAR(4)
 Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C32A)=
 Sof(H32C)=Sof(H32D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=FVAR(4)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C37)=Sof(H37A)=Sof(H37B)=1-FVAR(5)
 Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=
 Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=FVAR(5)
 Fixed Sof: O4(0.5) C38(0.5) H38A(0.5) H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5)
 C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(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)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C3(H3), C10(H10), C20A(H20A), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C27(H27C,H27D), C29A(H29A,H29B), C28A(H28A,H28B), C31(H31A,
 H31B), C30(H30A,H30B), C34(H34A,H34B), C36(H36A,H36B), C35(H35A,H35B),
 C32(H32A,H32B), C26A(H26A,H26B), C37(H37A,H37B), C33(H33A,H33B), C29(H29C,
 H29D), C28(H28C,H28D), C26(H26C,H26D), C33A(H33C,H33D), C30A(H30C,H30D),
 C32A(H32C,H32D), C31A(H31C,H31D), C34A(H34C,H34D), C35A(H35C,H35D), C36A(H36C,
 H36D), C37A(H37C,H37D), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C45(H45A,H45B), C44(H44A,H44B), C43(H43A,H43B), C42(H42A,H42B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C6(H6), C16(H16), C5(H5), C7(H7), C17(H17), C18(H18)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C2(H2A,H2B,H2C), C25(H25A,H25B,H25C), C1(H1A,H1B,H1C),
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C22A(H22A,H22B,H22C), C21A(H21A,H21B,
 H21C), C22(H22D,H22E,H22F), C21(H21D,H21E,H21F)
;
_shelx_res_checksum              25959
_shelx_hkl_checksum              91865
_olex2_submission_special_instructions 'No special instructions were received'