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_7129072
_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         'C25 H31 F4 Gd I2 N2 O3'
_chemical_formula_sum            'C25 H31 F4 Gd I2 N2 O3'
_chemical_formula_weight         894.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-09-07
_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                 91.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.811(3)
_cell_length_b                   9.4750(19)
_cell_length_c                   23.728(5)
_cell_measurement_reflns_used    5045
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2878.8(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32403
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.503
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.6
_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    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.00188(8)
_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   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0335
_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^)+39.5165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4716
_reflns_number_total             5045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_original_cell_volume        2878.8(10)
_cod_database_code               7129072
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C19, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C19 \\sim C18: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C24 \\sim C25: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C14(H14A,H14B), C18(H18A,H18B), C16(H16A,H16B), C22(H22A,
 H22B), C25(H25A,H25B), C17(H17A,H17B), C20(H20A,H20B), C24(H24A,H24B),
 C15(H15A,H15B), C23(H23A,H23B), C19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C12(H12), C10(H10), C2(H2), C11(H11), C3(H3), C4(H4)
;
_shelx_res_checksum              85751
_shelx_hkl_checksum              67434
_olex2_submission_special_instructions 'No special instructions were received'