Synthesis and characterization of rare-earth metallate amido complexes bearing 2-amidate-functionalized indolyl ligand and their application in the hydroboration of esters with pinacolborane
Wei, Yun; Bao, Qin; Song, Lulu; Hong, Dongjing; Gao, Jianjian; Wang, Shaowu; Zhu, Xiancui; Zhou, Shuangliu; Mu, Xiaolong; Dalton Transactions  (2022) –; doi:10.1039/D1DT03384K

data_7709354
_publ_section_title
;
 Synthesis and characterization of rare-earth metallate amido complexes
 bearing 2-amidate-functionalized indolyl ligand and their application in
 the hydroboration of esters with pinacolborane
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03384K
_journal_year                    2022
_chemical_formula_moiety         'C81 H120 Cl Dy3 N9 O3 Si6, C16 H32 Li O4'
_chemical_formula_sum            'C97 H152 Cl Dy3 Li N9 O7 Si6'
_chemical_formula_weight         2254.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                67.638(2)
_cell_angle_beta                 83.935(2)
_cell_angle_gamma                61.667(2)
_cell_formula_units_Z            2
_cell_length_a                   19.827(3)
_cell_length_b                   20.177(3)
_cell_length_c                   21.529(3)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      24.898
_cell_measurement_theta_min      2.183
_cell_volume                     6981.1(18)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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  0.0905
_diffrn_reflns_av_unetI/netI     0.1395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            81915
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_min         1.027
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1206 before and 0.0561 after correction. The Ratio of minimum to maximum transmission is 0.6304. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             2310
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.804
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         31769
_refine_ls_number_restraints     362
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1751
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14621
_reflns_number_total             31769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03384k2.cif
_cod_data_source_block           1d
_cod_database_code               7709354
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_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
 O6-C90 = O6-C93 = O4-C82 = O4-C85 = O7-C94 = O7-C97 = O5-C86 = O5-C89
 1.43 with sigma of 0.01
 C91-C90 = C91-C92 = C92-C93 = C83-C82 = C83-C84 = C85-C84 = C94-C95 = C96-C95
 = C97-C96 = C87-C86 = C88-C87 = C88-C89
 1.54 with sigma of 0.01
 C59-C58 = C60-C58 = C42-C40 = C41-C40
 1.54 with sigma of 0.01
 C86-C88 = C89-C87 = C97-C95 = C96-C94 = C85-C83 = C84-C82 = C93-C91 = C92-C90
 2.52 with sigma of 0.01
 C60-C59 = C42-C41
 2.52 with sigma of 0.02
 O7-Li3I \\sim O5-Li3I \\sim O4-Li3I \\sim O6-Li3I
 with sigma of 0.02
 O7-O4 \\sim O7-O6 \\sim O7-O5 \\sim O4-O6 \\sim O4-O5 \\sim O6-O5
 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
4. Uiso/Uaniso restraints and constraints
C53 \\sim C58 \\sim C59 \\sim C60: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C96) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Li3I, O4, C82, C85, C83, C84, O7, O6, O5, C94, C97, C90, C93, C86, C89, C95,
 C96, C91, C92, C87, C88
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C58, C60, C59, C53, C36, C40, C41, C42, C35, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C37(H37), C40(H40), C58(H58), C61(H61)
6.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,
 H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B),
 C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
  C96(H96A,H96B), C97(H97A,H97B)
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),
 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)
6.d Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15), C31(C32,C33,C34,C35,C36), C52(C53,C54,C55,C56,C57)
6.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), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C)
;
_shelx_res_checksum              31035
_shelx_hkl_checksum              23113
_shelx_fab_checksum              6069
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'