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_7129078
_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         'C23 H31 Eu I2 N3 O2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C25 H35 Eu I2 N3 O2.5'
_chemical_formula_weight         823.32
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-01
_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                120
_cell_formula_units_Z            18
_cell_length_a                   18.997(3)
_cell_length_b                   18.997(3)
_cell_length_c                   43.447(9)
_cell_measurement_reflns_used    3473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     13579(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            51472
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.553
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    4.150
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.6425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       prism
_exptl_crystal_F_000             7110
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.000227(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0693P)^2^+39.8606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2247
_reflns_number_total             2669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           1_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_original_cell_volume        13578(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C25 H35 Eu I2 N3 O2.50'
_cod_database_code               7129078
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Shared sites
{N2, O1}
{N3, O2}
2. Restrained distances
 O3-C13 = O3-C16
 1.44 with sigma of 0.02
 C13-C14 = C15-C16
 1.53 with sigma of 0.02
 C14-C15
 1.54 with sigma of 0.02
 O3-C14 = O3-C15 = C13-C15 = C14-C16
 2.38 with sigma of 0.04
 C14-C16 \\sim C13-C15
 with sigma of 0.04
 O3-C14 \\sim O3-C15
 with sigma of 0.04
 C13-C14 \\sim C14-C15 \\sim C15-C16
 with sigma of 0.02
 O3-C13 \\sim O3-C16
 with sigma of 0.02
3. Rigid bond restraints
 C6A, C1A, C2A, C3A, C7A, C4A, C8A, C5A, C9A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C6, C2, C7, C3, C8, C4, C5, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O3 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1A \\sim C6A \\sim C2A \\sim C3A \\sim C7A \\sim C4A \\sim C8A \\sim C5A \\sim
C9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C12 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
C6 \\sim C1 \\sim C2 \\sim C7 \\sim C3 \\sim C8 \\sim C4 \\sim C5 \\sim C9:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
Uanis(N2) = Uanis(O1)
Uanis(N3) = Uanis(O2)
5. Rigid body (RIGU) restrains
 O3, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I1)=1-FVAR(1)
 Sof(I1A)=FVAR(1)
 Sof(N3)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=
 Sof(H2A)=Sof(C1A)=Sof(H1A)=1-FVAR(2)
 Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(N2)=FVAR(2)
 Sof(O2)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(3)
 Sof(O1)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(3)
 Fixed Sof: O3(0.25) C13(0.25) H13A(0.25) H13B(0.25) C14(0.25) H14A(0.25)
 H14B(0.25) C15(0.25) H15A(0.25) H15B(0.25) C16(0.25) H16A(0.25) H16B(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C16(H16A,H16B), C9A(H9AA,H9AB), C7A(H7AA,H7AB),
 C8A(H8AA,H8AB), C6A(H6AA,H6AB)
7.b Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A), C1A(H1A), C10(H10), C11(H11),
 C12(H12), C2(H2), C1(H1), C3(H3), C4(H4), C5(H5)
;
_shelx_res_checksum              25675
_shelx_hkl_checksum              66897
_olex2_submission_special_instructions 'No special instructions were received'