Volatile lanthanide complexes with fluorinated heptadentate ligands.
Zgrabik, Joshua C.; Bhuniya, Balaka; Branstad Phillips, Thomas; Barroso, Jorge; Vlaisavljevich, Bess; Daly, Scott R.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2998–3009; doi:10.1039/d3dt04198k

data_7715364
_publ_section_title
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 Volatile lanthanide complexes with fluorinated heptadentate ligands.
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_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2998
_journal_page_last               3009
_journal_paper_doi               10.1039/d3dt04198k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H14 F30 N4 O3 Yb'
_chemical_formula_sum            'C27 H14 F30 N4 O3 Yb'
_chemical_formula_weight         1185.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
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_audit_update_record
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2023-12-12 deposited with the CCDC.	2024-01-12 downloaded from the CCDC.
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_cell_angle_alpha                89.530(5)
_cell_angle_beta                 86.742(5)
_cell_angle_gamma                86.666(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0912(10)
_cell_length_b                   10.4385(10)
_cell_length_c                   17.6508(18)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.312
_cell_volume                     1853.1(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex'
_diffrn_measurement_method       'CCD Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56905
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         2.025
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0574 before and 0.0397 after correction.
The Ratio of minimum to maximum transmission is 0.9069.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_description       prism-like
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.615
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         7590
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0390P)^2^+4.5250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7419
_reflns_number_total             7590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04198k2.cif
_cod_data_source_block           dal2127
_cod_database_code               7715364
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C36-F31A = C36-F31B = C36-F32A = C36-F32B = C37-F33A = C37-F33B = C37-F34A =
 C37-F34B
 1.36522 with sigma of 0.02
 C38-F35A = C38-F36A = C38-F37A = C38-F35B = C38-F36B = C38-F37B
 1.33054 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F31A \\sim F32A \\sim F33A \\sim F34A \\sim F35A \\sim F36A \\sim F37A \\sim
F31B \\sim F32B \\sim F33B \\sim F34B \\sim F35B \\sim F36B \\sim F37B \\sim
C36 \\sim C37 \\sim C38: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 F31A, F32A, F33A, F34A, F35A, F36A, F37A, F31B, F32B, F33B, F34B, F35B, F36B,
 F37B, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F31B)=Sof(F32B)=Sof(F33B)=Sof(F34B)=Sof(F35B)=Sof(F36B)=Sof(F37B)=1-FVAR(1)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=Sof(F35A)=Sof(F36A)=Sof(F37A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C21(H21A,H21B), C31(H31A,H31B), C32(H32A,H32B)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C24(H24), C34(H34)
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_shelx_res_checksum              44948
_olex2_submission_special_instructions 'No special instructions were received'