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_7700320
_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         'C68 H70 N8 Y2'
_chemical_formula_sum            'C68 H70 N8 Y2'
_chemical_formula_weight         1177.14
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 106.16
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.995(3)
_cell_length_b                   20.995(5)
_cell_length_c                   23.338(6)
_cell_measurement_reflns_used    5926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.698
_cell_measurement_theta_min      2.292
_cell_volume                     6116(3)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1758
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.632
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10794
_refine_ls_number_restraints     1572
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1079P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4939
_reflns_number_total             10794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01582e2.cif
_cod_data_source_block           140617b
_cod_depositor_comments
'Adding full bibliography for 7700314--7700321.cif.'
_cod_database_code               7700320
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.787
_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. Rigid bond restraints
 C44, C45, C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C10, C11, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C44 \\sim C45 \\sim C46 \\sim C47: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.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), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C49(H49),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C64(H64), C65(H65), C66(H66),
  C67(H67), C68(H68)
4.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), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              4433
_olex2_submission_special_instructions 'No special instructions were received'