Yttrium and Aluminum Alkyl Complexes of a Rigid Bis-Anilido NON-Donor Ligand: Synthesis and Hydroamination Catalysis
Motolko, Kelly S. A.; Emslie, David J. H.; Jenkins, Hilary A.; Organometallics 36 (2017) 1601–; doi:10.1021/acs.organomet.7b00156

data_4089281
_publ_section_title
;
 Yttrium and Aluminum Alkyl Complexes of a Rigid Bis-Anilido NON-Donor
 Ligand: Synthesis and Hydroamination Catalysis
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1601
_journal_paper_doi               10.1021/acs.organomet.7b00156
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C61 H93 N2 O2 Si Y, C6 H18 O Si2'
_chemical_formula_sum            'C67 H111 N2 O3 Si3 Y'
_chemical_formula_weight         1165.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.291(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.029(2)
_cell_length_b                   14.7584(12)
_cell_length_c                   20.3216(17)
_cell_measurement_reflns_used    5969
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.12
_cell_measurement_theta_min      2.25
_cell_volume                     6917.3(10)
_computing_cell_refinement       '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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1083
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64960
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.419
_diffrn_reflns_theta_min         1.730
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0616 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8609. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       rod
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12729
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0554P)^2^+2.0520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8143
_reflns_number_total             12729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00156_si_002.cif
_cod_data_source_block           km3
_cod_database_code               4089281
_shelx_shelxl_version_number     2014/7
_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. Uiso/Uaniso restraints and constraints
Uanis(Si2) = Uanis(Si3) = Uanis(Si2A) = Uanis(Si3A)
Uanis(C67) = Uanis(C63)
Uanis(C65) = Uanis(C64)
Uanis(C66) = Uanis(C62)
Uanis(C66A) = Uanis(C62A)
Uanis(C64A) = Uanis(C65A)
Uanis(C67A) = Uanis(C63A)
3. Rigid body (RIGU) restrains
 C64A, Si2A, O3A, C62A, C63A, Si3A, C65A, C66A, C67A, Si2A, O3A, Si2A, C62A,
 Si2A, C63A, Si2A, C64A, Si3A, O3A, Si3A, C65A, Si3A, C66A, Si3A, C67A, C64,
 Si2, O3, C62, C63, Si3, C65, C66, C67, Si2, O3, Si2, C62, Si2, C63, Si2, C64,
 Si3, O3, Si3, C65, Si3, C66, Si3, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Si2A, Si3A, O3A, C62A, C63A, C64A, C65A, C66A, C67A} sigma for 1-2: 0.001,
1-3: 0.002
as
{Si2, Si3, O3, C62, C63, C64, C65, C66, C67}
5. Others
 Fixed Sof: Si2(0.5) Si3(0.5) O3(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
 C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5)
 C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) Si2A(0.5) Si3A(0.5) O3A(0.5) C62A(0.5)
 H62D(0.5) H62E(0.5) H62F(0.5) C63A(0.5) H63D(0.5) H63E(0.5) H63F(0.5)
 C64A(0.5) H64D(0.5) H64E(0.5) H64F(0.5) C65A(0.5) H65D(0.5) H65E(0.5)
 H65F(0.5) C66A(0.5) H66D(0.5) H66E(0.5) H66F(0.5) C67A(0.5) H67D(0.5)
 H67E(0.5) H67F(0.5)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C36(H36), C45(H45), C48(H48), C51(H51)
6.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
6.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C62A(H62D,H62E,H62F), C63A(H63D,H63E,H63F), C64A(H64D,H64E,H64F), C65A(H65D,
 H65E,H65F), C66A(H66D,H66E,H66F), C67A(H67D,H67E,H67F)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C8(H8), C26(H26), C28(H28), C41(H41), C43(H43)
;
_shelx_res_checksum              35020
_shelx_hkl_checksum              53490
_olex2_submission_special_instructions 'No special instructions were received'