Yttrium Dialkyl Supported by a Silaamidinate Ligand: Synthesis, Structure and Catalysis on Cyclotrimerization of Isocyanates
Liu, Deshuai; Zhou, Dahai; Yang, Hao; Li, Jianfeng; Cui, Chunming; Chemical Communications  (2019) –; doi:10.1039/C9CC06282C

data_7124196
_publ_section_title
;
 Yttrium Dialkyl Supported by a Silaamidinate Ligand: Synthesis, Structure
 and Catalysis on Cyclotrimerization of Isocyanates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06282C
_journal_year                    2019
_chemical_formula_moiety         'C47 H79 N4 Si3 Y'
_chemical_formula_sum            'C47 H79 N4 Si3 Y'
_chemical_formula_weight         873.32
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-11 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.91(3)
_cell_angle_beta                 72.79(3)
_cell_angle_gamma                87.15(3)
_cell_formula_units_Z            2
_cell_length_a                   11.665(2)
_cell_length_b                   12.804(3)
_cell_length_c                   19.310(4)
_cell_measurement_reflns_used    5424
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8664
_cell_measurement_theta_min      1.6267
_cell_volume                     2693.6(11)
_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      113.1500
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25678
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.780
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0894P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6752
_reflns_number_total             9430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06282c2.cif
_cod_data_source_block           lds
_cod_database_code               7124196
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C41, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0001
3.a Ternary CH refined with riding coordinates:
 C8(H8), C9(H9), C7(H7), C6(H6)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C44(H44), C37(H37), C42(H42), C39(H39), C32(H32), C43(H43),
 C35(H35), C38(H38), C34(H34), C33(H33)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C30(H30A,
 H30B,H30C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              21868
_shelx_fab_checksum              15770
_olex2_submission_special_instructions 'No special instructions were received'