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_7049280
_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         'C68 H84 N6 O6 Si2 Yb2'
_chemical_formula_sum            'C68 H84 N6 O6 Si2 Yb2'
_chemical_formula_weight         1483.67
_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                112.592(4)
_cell_angle_beta                 91.520(5)
_cell_angle_gamma                110.684(5)
_cell_formula_units_Z            1
_cell_length_a                   11.095(4)
_cell_length_b                   14.589(6)
_cell_length_c                   16.114(6)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.21
_cell_volume                     2212.8(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21550
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.711
_diffrn_reflns_theta_min         1.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1349 before and 0.0755 after correction. The Ratio of minimum to maximum transmission is 0.5543. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             750
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.153
_refine_diff_density_min         -3.401
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     679
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6607
_reflns_number_total             8258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00507b2.cif
_cod_data_source_block           2eb
_cod_depositor_comments
'Adding full bibliography for 7049263--7049284.cif.'
_cod_database_code               7049280
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.635
_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
 C32-C33
 1.5 with sigma of 0.02
 C33-C34
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C26, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O3, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N2, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Yb1, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.007
 N1, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N3, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N3, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C22, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Yb1 \\sim C26: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.007
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: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Si1) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              70024
_shelx_fab_checksum              18536
_olex2_submission_special_instructions 'No special instructions were received'