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_7049274
_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         '2(C37 H43 N2 O3 Yb)'
_chemical_formula_sum            'C74 H86 N4 O6 Yb2'
_chemical_formula_weight         1473.54
_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                79.527(2)
_cell_angle_beta                 76.232(2)
_cell_angle_gamma                89.163(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8086(16)
_cell_length_b                   16.837(2)
_cell_length_c                   20.863(3)
_cell_measurement_reflns_used    7075
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.97
_cell_measurement_theta_min      2.19
_cell_volume                     4295.3(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       '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 0.992
_diffrn_measured_fraction_theta_max 0.988
_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  0.0788
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43638
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.409
_diffrn_reflns_theta_min         1.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         15663
_refine_ls_number_restraints     1768
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0843P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7621
_reflns_number_total             15663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00507b2.cif
_cod_data_source_block           1ea
_cod_depositor_comments
'Adding full bibliography for 7049263--7049284.cif.'
_cod_original_cell_volume        4295.1(9)
_cod_database_code               7049274
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.631
_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
 C72-C73 = C35-C36 = C68-C69 = C71-C72 = C19-C21 = C30-C31 = C31-C32 = C67-C68
 1.54 with sigma of 0.01
3. Rigid bond restraints
 C27, C28, C28, C29, O6, C74, C50, C51, C65, C66, C73, C74, C34, C35, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C49, C50, C61, C62, C56, C58, C63, C64, C24, C29, C26, C27, O6, C71, C72, C73
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C52, C56, C59, C60, C61, C66, C69, C70, C53, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N2, C9, O5, C70, O5, C67, O3, C37, O4, C46, O3, C34, C16, C17, N3, C45, C19,
 C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\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 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: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O3) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(O5) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(O6) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73)
\\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C53(H53), C56(H56)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C67(H67A,H67B),
 C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
  C73(H73A,H73B), C74(H74A,H74B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C2(H2), C4(H4), C5(H5),
 C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C49(H49), C50(H50), C51(H51), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66)
5.d Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C28,C29), C61(C62,C63,C64,C65,C66)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C)
;
_shelx_res_checksum              97891
_shelx_fab_checksum              48277
_olex2_submission_special_instructions 'No special instructions were received'