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_7715361
_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         'C21 H15 F18 N4 O3 Yb'
_chemical_formula_sum            'C21 H15 F18 N4 O3 Yb'
_chemical_formula_weight         886.41
_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     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
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2023-12-12 deposited with the CCDC.	2024-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.043(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1775(18)
_cell_length_b                   10.2981(10)
_cell_length_c                   17.0455(17)
_cell_measurement_reflns_used    36260
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.383
_cell_volume                     2866.8(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.318
_diffrn_reflns_theta_min         2.660
_exptl_absorpt_coefficient_mu    3.412
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0828 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.7414.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       'colorless plate-like'
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       0.00077(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4094
_reflns_number_total             5785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04198k2.cif
_cod_data_source_block           dal2071
_cod_database_code               7715361
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.477
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C21(H21A,H21B), C22(H22A,H22B), C31(H31A,
 H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C24(H24), C34(H34)
;
_shelx_res_checksum              72576
_olex2_submission_special_instructions 'No special instructions were received'