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_1570854
_publ_section_title
;
 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         'C49 H73 Al N3 Y'
_chemical_formula_sum            'C49 H66 Al N3 Y'
_chemical_formula_weight         812.93
_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                 99.503(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4571(12)
_cell_length_b                   19.681(3)
_cell_length_c                   21.041(3)
_cell_measurement_reflns_used    6785
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.907
_cell_measurement_theta_min      2.291
_cell_volume                     4679.4(11)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1745
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            92292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         1.963
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0849 before and 0.0711 after correction. The Ratio of minimum to maximum transmission is 0.9315. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.5352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6014
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06599e2.cif
_cod_data_source_block           mo_210917a_a
_cod_depositor_comments
'Adding full bibliography for 1570851--1570856.cif.'
_cod_original_cell_volume        4679.6(10)
_cod_database_code               1570854
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.829
_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
 C1-C2 = C1'-C2'
 1.53 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(C2')
\\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms
of 0.04
4. Others
 Sof(C1')=Sof(H1'1)=Sof(H1'2)=Sof(C2')=Sof(H2'1)=Sof(H2'2)=Sof(H2'3)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1'(H1'1,H1'2), C5(H5A,H5B), C7(H7A,H7B), C36(H36A,H36B),
 C43(H43A,H43B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C48(H48),
  C49(H49)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2'(H2'1,H2'2,H2'3), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'