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_7049263
_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 H98 Gd2 N4 O6 Si2'
_chemical_formula_sum            'C66 H98 Gd2 N4 O6 Si2'
_chemical_formula_weight         1414.16
_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                 97.0820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9048(10)
_cell_length_b                   17.2036(15)
_cell_length_c                   17.5111(15)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.20
_cell_volume                     3559.0(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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  0.1049
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39748
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         1.666
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+5.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5887
_reflns_number_total             8153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00507b2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7049263--7049284.cif.'
_cod_database_code               7049263
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.676
_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
 C23-C24 \\sim C24-C25 \\sim C25-C23 \\sim C23'-C24' \\sim C24'-C25' \\sim
C25'-C23'
 with sigma of 0.02
 Si1-C23 \\sim Si1-C24 \\sim Si1-C25 \\sim Si1-C23' \\sim Si1-C24' \\sim
Si1-C25'
 with sigma of 0.02
3. Rigid bond restraints
 O2, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O3, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si1, C22, C23, C24, C25, C23', C24', C25'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O2 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O3 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Si1 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C23' \\sim C24' \\sim C25':
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19)
6.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C23'(H23D,H23E,H23F), C24'(H24D,H24E,H24F), C25'(H25D,H25E,H25F)
;
_shelx_res_checksum              266
_olex2_submission_special_instructions 'No special instructions were received'