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_7049266
_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         'C66 H92 N6 O6 Y2'
_chemical_formula_sum            'C66 H92 N6 O6 Y2'
_chemical_formula_weight         1243.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 90.1120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4194(11)
_cell_length_b                   15.3671(15)
_cell_length_c                   18.6412(18)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.18
_cell_volume                     3271.2(5)
_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    'ShelXT (Sheldrick, 2015)'
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32723
_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         25.450
_diffrn_reflns_theta_min         1.717
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6048
_refine_ls_number_restraints     729
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0489P)^2^+1.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4573
_reflns_number_total             6048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00507b2.cif
_cod_data_source_block           1cc
_cod_depositor_comments
'Adding full bibliography for 7049263--7049284.cif.'
_cod_database_code               7049266
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C27
 1.5 with sigma of 0.02
 C28-C29
 1.5 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.02
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 C27A \\sim C28 \\sim C28A \\sim C29 \\sim C30 \\sim
C31 \\sim C32 \\sim C33 \\sim C32A: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27A)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C29) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=
 Sof(H28D)=Sof(H29C)=Sof(H29D)=Sof(H31C)=Sof(H31D)=Sof(H33C)=Sof(H33D)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H29A)=Sof(H29B)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H33A)=
 Sof(H33B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C26(H26A,H26B), C26(H26C,H26D), C27(H27A,H27B), C27A(H27C,
 H27D), C28(H28A,H28B), C28A(H28C,H28D), C29(H29A,H29B), C29(H29C,H29D),
 C30(H30A,H30B), C31(H31A,H31B), C31(H31C,H31D), C32(H32A,H32B), C33(H33A,H33B),
  C33(H33C,H33D), C32A(H32C,H32D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C24(H24)
5.d X=CH2 refined with riding coordinates:
 C25(H25A,H25B)
5.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              52830
_olex2_submission_special_instructions 'No special instructions were received'