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_7129077
_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         'C39 H35 F8 N4 Nd O2, C4 H8 O'
_chemical_formula_sum            'C43 H43 F8 N4 Nd O3'
_chemical_formula_weight         960.05
_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
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-05-11 deposited with the CCDC.	2021-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.82(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.141(4)
_cell_length_b                   10.909(2)
_cell_length_c                   38.732(8)
_cell_measurement_reflns_used    2047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     8078(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            94237
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.683
_diffrn_reflns_theta_min         1.053
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.368
_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    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.872
_exptl_transmission_factor_min   0.782
_refine_diff_density_max         7.202
_refine_diff_density_min         -1.948
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1076
_refine_ls_number_reflns         15170
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1476P)^2^+30.6956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12360
_reflns_number_total             15170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04080d2.cif
_cod_data_source_block           1_a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7129070--7129084.cif.'
_cod_database_code               7129077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.772
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C80) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(C86) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C85) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C41A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C41A) = Uanis(C41)
3. Rigid body (RIGU) restrains
 C80, O5, C79, C82, C81, C83, O6, C86, C84, C85
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C40, C41, C42, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H40C)=Sof(H40D)=Sof(H42C)=Sof(H42D)=Sof(C41A)=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H42A)=Sof(H42B)=FVAR(1)
 Fixed Sof: H45A(0.5) H45B(0.5) H45C(0.5) H45D(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H47A(0.5) H47B(0.5) H47C(0.5) H47D(0.5) C46A(0.5) H46C(0.5) H46D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C40(H40A,H40B), C40(H40C,H40D), C41(H41A,H41B),
 C42(H42A,H42B), C42(H42C,H42D), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C45(H45C,H45D), C46(H46A,H46B), C47(H47A,H47B), C47(H47C,H47D), C79(H79A,
 H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C46A(H46C,H46D), C41A(H41C,
 H41D)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C22(H22),
 C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C48(H48), C51(H51), C52(H52), C53(H53),
 C57(H57), C58(H58), C59(H59), C61(H61), C64(H64), C65(H65), C66(H66), C70(H70),
  C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
;
_shelx_res_checksum              71737
_shelx_hkl_checksum              38375
_olex2_submission_special_instructions 'No special instructions were received'