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_7715362
_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         'C30 H35 F21 N4 O3'
_chemical_formula_sum            'C30 H35 F21 N4 O3'
_chemical_formula_weight         898.62
_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             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
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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.
;
_cell_angle_alpha                102.461(5)
_cell_angle_beta                 98.735(5)
_cell_angle_gamma                115.475(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9357(12)
_cell_length_b                   13.2583(13)
_cell_length_c                   14.1754(14)
_cell_measurement_reflns_used    2576
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.944
_cell_measurement_theta_min      2.323
_cell_volume                     1899.7(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Duo with Photon 3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         1.967
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0588 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.9666.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0454P)^2^+1.0778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5152
_reflns_number_total             7792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04198k2.cif
_cod_data_source_block           dal2123
_cod_original_cell_volume        1899.7(3)
_cod_database_code               7715362
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F33-C29 \\sim F33A-C29A
 with sigma of 0.01
 F34-C29 \\sim F34A-C29A
 with sigma of 0.01
 C28-C29 \\sim C28-C29A
 with sigma of 0.01
 F33-F34 \\sim F33A-F34A
 with sigma of 0.01
 F33-C28 \\sim F33A-C28
 with sigma of 0.01
 F34-C28 \\sim F34A-C28
 with sigma of 0.01
 F36-C30 \\sim F36A-C30
 with sigma of 0.01
 F35-C30 \\sim F35A-C30
 with sigma of 0.01
 C30-F37 \\sim C30-F37A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F35 \\sim F36 \\sim F37 \\sim F35A \\sim F36A \\sim F37A \\sim C30: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
F33 \\sim F34 \\sim F33A \\sim F34A \\sim C29 \\sim C29A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 2A
F25A \\sim F26A \\sim F27A \\sim C22 \\sim F25B \\sim F26B \\sim F27B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 F35, F36, F37, F35A, F36A, F37A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F33, F34, F33A, F34A, C29, C29A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F25A, F26A, F27A, C22, F25B, F26B, F27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C29A)=Sof(F33A)=Sof(F34A)=Sof(F35A)=Sof(F36A)=Sof(F37A)=1-FVAR(1)
 Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=Sof(F37)=Sof(C29)=FVAR(1)
 Sof(F25B)=Sof(F26B)=Sof(F27B)=1-FVAR(2)
 Sof(F25A)=Sof(F26A)=Sof(F27A)=FVAR(2)
6.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)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C8(H8), C18(H18)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
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_shelx_res_checksum              98263
_olex2_exptl_crystal_mounting_method 'MiTeGen 100 micron MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'