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_7715365
_publ_section_title
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 Volatile lanthanide complexes with fluorinated heptadentate ligands.
;
_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         'C21 H24 F9 N4 O3 Yb, C4 H10 O'
_chemical_formula_sum            'C25 H34 F9 N4 O4 Yb'
_chemical_formula_weight         798.60
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-12 deposited with the CCDC.	2024-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7260(19)
_cell_length_b                   19.9703(19)
_cell_length_c                   15.5564(15)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.424
_cell_volume                     6128.2(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            106067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         1.954
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0721 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8585.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.434
_refine_diff_density_min         -2.355
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0379
_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^)+54.2407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5488
_reflns_number_total             6289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04198k2.cif
_cod_data_source_block           dal2161
_cod_database_code               7715365
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.602
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C31(H31A,H31B), C32(H32A,H32B), C21(H21A,
 H21B), C22(H22A,H22B), C43(H43A,H43B), C42(H42A,H42B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C34(H34), C24(H24)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C27(H27A,H27B,H27C), C41(H41A,H41B,
 H41C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              50634
_olex2_submission_special_instructions 'No special instructions were received'