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_1570855
_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 H71 Al Lu N3'
_chemical_formula_sum            'C49 H73 Al Lu N3'
_chemical_formula_weight         906.05
_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                 99.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4749(4)
_cell_length_b                   19.6122(7)
_cell_length_c                   20.9790(9)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.675
_cell_measurement_theta_min      2.224
_cell_volume                     4662.0(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1165
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            111964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9667
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7624
_reflns_number_total             9667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06599e2.cif
_cod_data_source_block           mo_210806a_a
_cod_depositor_comments
'Adding full bibliography for 1570851--1570856.cif.'
_cod_database_code               1570855
_shelx_shelxl_version_number     2018/3
_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
 C49-C48 = C49'-C48'
 1.53 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
C48 \\sim C48': within 2A with sigma of 0.02 and sigma for terminal atoms of
0.05
Uanis(C49) \\sim Ueq, Uanis(C49') \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C48) \\sim Ueq, Uanis(C48') \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Sof(C48')=Sof(H48c)=Sof(H48d)=Sof(C49')=Sof(H49d)=Sof(H49e)=Sof(H49f)=1-FVAR(1)
 Sof(C48)=Sof(H48a)=Sof(H48b)=Sof(C49)=Sof(H49a)=Sof(H49b)=Sof(H49c)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C34(H34), C37(H37)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C21(H21a,H21b), C44(H44a,H44b), C46(H46a,H46b), C48(H48a,
 H48b), C48'(H48c,H48d)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c), C13(H13a,H13b,
 H13c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,
 H39b,H39c), C41(H41a,H41b,H41c), C43(H43a,H43b,H43c), C45(H45a,H45b,H45c),
 C47(H47a,H47b,H47c), C49(H49a,H49b,H49c), C49'(H49d,H49e,H49f)
;
_olex2_submission_special_instructions 'No special instructions were received'