Synthesis, characterization, and reactivity of dinuclear organo-rare-earth-metal alkyl complexes supported by 2-amidate-functionalized indolyl ligands: substituent effects on coordination and reactivity.
Hong, Dongjing; Zhu, Xiancui; Wang, Shaowu; Wei, Yun; Zhou, Shuangliu; Huang, Zeming; Zhu, Shan; Wang, Ruru; Yue, Wenrun; Mu, Xiaolong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5230–5242; doi:10.1039/c9dt00507b

data_7049275
_publ_section_title
;
 Synthesis, characterization, and reactivity of dinuclear
 organo-rare-earth-metal alkyl complexes supported by
 2-amidate-functionalized indolyl ligands: substituent effects on
 coordination and reactivity.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5230
_journal_page_last               5242
_journal_paper_doi               10.1039/c9dt00507b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C103 H106 N14 O3 Yb2'
_chemical_formula_sum            'C103 H106 N14 O3 Yb2'
_chemical_formula_weight         1934.09
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-27 deposited with the CCDC.    2019-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                101.4710(10)
_cell_angle_beta                 96.2690(10)
_cell_angle_gamma                93.2780(10)
_cell_formula_units_Z            2
_cell_length_a                   14.7004(8)
_cell_length_b                   14.9519(9)
_cell_length_c                   23.7312(14)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.38
_cell_volume                     5064.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0916
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52092
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         1.394
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.562
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         18488
_refine_ls_number_restraints     2344
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13281
_reflns_number_total             18488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00507b2.cif
_cod_data_source_block           1ef
_cod_depositor_comments
'Adding full bibliography for 7049263--7049284.cif.'
_cod_database_code               7049275
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.671
_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. Rigid bond restraints
 N4, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N14, C97
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C98, C103
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N9, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N13, C94
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C61, C63
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C100, C101
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C58, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C61, C62
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C98, C99
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim 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 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40), C58(H58), C61(H61)
4.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C77(H77A,H77B), C87(H87A,H87B), C97(H97A,H97B)
4.c Aromatic/amide H refined with riding coordinates:
 C99(H99), C100(H100), C101(H101), C102(H102), C103(H103), C2(H2), C4(H4),
 C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C23(H23), C25(H25),
 C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C44(H44), C46(H46),
  C47(H47), C48(H48), C49(H49), C54(H54), C55(H55), C56(H56), C64(H64),
 C65(H65), C66(H66), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96)
4.d Fitted hexagon refined as free rotating group:
 C98(C99,C100,C101,C102,C103)
4.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C)
;
_shelx_res_checksum              95355
_shelx_fab_checksum              98195
_olex2_submission_special_instructions 'No special instructions were received'