Rare-earth metal ethylene and ethyne complexes.
Jiang, Wen; Rajeshkumar, Thayalan; Guo, Mengyue; Lin, Yuejian; Maron, Laurent; Zhang, Lixin; Chemical science 15 (2024) 3495–3501; doi:10.1039/d3sc06599e

data_1570856
_publ_section_title
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 Rare-earth metal ethylene and ethyne complexes.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3495
_journal_page_last               3501
_journal_paper_doi               10.1039/d3sc06599e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C55 H88 Al2 N3 Y)'
_chemical_formula_sum            'C110 H176 Al4 N6 Y2'
_chemical_formula_weight         1868.30
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-28 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5841(6)
_cell_length_b                   30.8815(9)
_cell_length_c                   16.1320(5)
_cell_measurement_reflns_used    9589
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.809
_cell_measurement_theta_min      4.141
_cell_volume                     10725.0(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            210709
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.497
_diffrn_reflns_theta_min         3.783
_exptl_absorpt_coefficient_mu    1.400
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1365 before and 0.0772 after correction. The Ratio of minimum to maximum transmission is 0.8267. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.752
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         20088
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+13.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17502
_reflns_number_total             20088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06599e2.cif
_cod_data_source_block           ga_230406h_a
_cod_depositor_comments
'Adding full bibliography for 1570851--1570856.cif.'
_cod_database_code               1570856
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.730
_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. Restrained distances
 H11A-H11B = H11C-H11D
 1.6 with sigma of 0.005
 C11-H11A = C11-H11B = C11'-H11C = C11'-H11D
 0.98 with sigma of 0.003
 C14-C13
 1.53 with sigma of 0.002
 C3-H3A = C3-H3B
 0.96 with sigma of 0.002
 C11-C12 = C11'-C12' = C61-C60 = C61'-C60'
 1.53 with sigma of 0.005
3. Rigid bond restraints
 C13, C14
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C11') \\sim Ueq, Uanis(C12') \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C61') \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C61) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C60) = Uanis(C60')
5. Others
 Sof(C60')=Sof(H60C)=Sof(H60D)=Sof(C61')=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Sof(C11')=Sof(H11C)=Sof(H11D)=Sof(C12')=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(2)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C36(H36), C39(H39), C79(H79), C82(H82), C91(H91), C94(H94)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C13(H13A,H13B), C15(H15A,H15B), C42(H42A,H42B),
 C49(H49A,H49B), C60(H60A,H60B), C60'(H60C,H60D), C62(H62A,H62B), C64(H64A,
 H64B), C68(H68A,H68B), C70(H70A,H70B), C97(H97A,H97B), C104(H10D,H10E)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C32(H32), C33(H33), C34(H34), C44(H44),
 C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C75(H75), C76(H76), C77(H77), C87(H87), C88(H88), C89(H89),
 C99(H99), C100(H100), C101(H101), C102(H102), C103(H103), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C12'(H12D,H12E,H12F), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C61(H61A,H61B,H61C), C61'(H61D,H61E,H61F), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,
 H96C)
;
_olex2_submission_special_instructions 'No special instructions were received'