Synthesis and characterization of 2-t-butylimino-functionalized indolyl rare-earth metal amido complexes for the catalytic addition of terminal alkynes to carbodiimides: the dimeric complexes with the alkynide species in the μ-η<sup>1</sup>:η<sup>2</sup> bonding modes.
Feng, Zhijun; Huang, Zeming; Wang, Shaowu; Wei, Yun; Zhou, Shuangliu; Zhu, Xiancui; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11094–11102; doi:10.1039/c9dt01582e

data_7700318
_publ_section_title
;
 Synthesis and characterization of 2-t-butylimino-functionalized indolyl
 rare-earth metal amido complexes for the catalytic addition of terminal
 alkynes to carbodiimides: the dimeric complexes with the alkynide species
 in the \m-\h<sup>1</sup>:\h<sup>2</sup> bonding modes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11094
_journal_page_last               11102
_journal_paper_doi               10.1039/c9dt01582e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C62 H78 N8 Si2 Yb2'
_chemical_formula_sum            'C62 H78 N8 Si2 Yb2'
_chemical_formula_weight         1337.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-10 deposited with the CCDC.    2019-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.3030(10)
_cell_angle_beta                 80.6500(10)
_cell_angle_gamma                61.7530(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6269(9)
_cell_length_b                   12.9123(10)
_cell_length_c                   22.4030(17)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.399
_cell_measurement_theta_min      2.301
_cell_volume                     3131.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         1.815
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.049
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1200 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.4911. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+3.4755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9534
_reflns_number_total             11514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01582e2.cif
_cod_data_source_block           test_0m_a
_cod_depositor_comments
'Adding full bibliography for 7700314--7700321.cif.'
_cod_database_code               7700318
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.581
_shelx_estimated_absorpt_t_min   0.541
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
3. Rigid body (RIGU) restrains
 C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C12A, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              5954
_olex2_submission_special_instructions 'No special instructions were received'