Long aliphatic chain derivatives of trigonal lanthanide complexes.
Zhou, Yiwei; Buch, Christian D.; Hansen, Steen H.; Piligkos, Stergios; Dalton transactions (Cambridge, England : 2003) 52 (2023) 8792–8799; doi:10.1039/d3dt01191g

data_7713261
_publ_section_title
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 Long aliphatic chain derivatives of trigonal lanthanide complexes.
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_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8792
_journal_page_last               8799
_journal_paper_doi               10.1039/d3dt01191g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C87 H144 N7 O3 Yb'
_chemical_formula_sum            'C87 H144 N7 O3 Yb'
_chemical_formula_weight         1509.12
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-30
_audit_creation_method
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2022-12-30 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.216(2)
_cell_angle_beta                 98.672(2)
_cell_angle_gamma                115.930(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4294(8)
_cell_length_b                   12.4635(8)
_cell_length_c                   30.023(2)
_cell_measurement_reflns_used    9092
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.436
_cell_measurement_theta_min      2.721
_cell_volume                     4115.0(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            118800
_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         25.682
_diffrn_reflns_theta_min         2.014
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1198 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8622.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             1618
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+3.1301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14430
_reflns_number_total             15615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01191g2.cif
_cod_data_source_block           1_YbL18
_cod_database_code               7713261
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.629
_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:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C12A(H12A,H12B), C13A(H13A,H13B), C14A(H14A,
 H14B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,H18B),
 C19A(H19A,H19B), C20A(H20A,H20B), C21A(H21A,H21B), C22A(H22A,H22B), C23A(H23A,
 H23B), C24A(H24A,H24B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B),
 C28A(H28A,H28B), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C12B(H12C,H12D), C13B(H13C,
 H13D), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,H17D),
 C18B(H18C,H18D), C19B(H19C,H19D), C20B(H20C,H20D), C21B(H21C,H21D), C22B(H22C,
 H22D), C23B(H23C,H23D), C24B(H24C,H24D), C25B(H25C,H25D), C26B(H26C,H26D),
 C27B(H27C,H27D), C28B(H28C,H28D), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C12C(H12E,
 H12F), C13C(H13E,H13F), C14C(H14E,H14F), C15C(H15E,H15F), C16C(H16E,H16F),
 C17C(H17E,H17F), C18C(H18E,H18F), C19C(H19E,H19F), C20C(H20E,H20F), C21C(H21E,
 H21F), C22C(H22E,H22F), C23C(H23E,H23F), C24C(H24E,H24F), C25C(H25E,H25F),
 C26C(H26E,H26F), C27C(H27E,H27F), C28C(H28E,H28F)
2.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C5B(H5B), C3C(H3C), C11A(H11A), C7A(H7A), C5A(H5A),
 C7B(H7B), C11B(H11B), C11C(H11C), C7C(H7C), C5C(H5C)
2.c Idealised Me refined as rotating group:
 C29A(H29A,H29B,H29C), C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C29B(H29D,
 H29E,H29F), C29C(H29G,H29H,H29I), C10C(H10G,H10H,H10I)
;
_shelx_res_checksum              89387
_shelx_hkl_checksum              26432
_olex2_submission_special_instructions 'No special instructions were received'