Versatile reactivities of rare-earth metal dialkyl complexes supported by a neutral pyrrolyl-functionalized β-diketiminato ligand.
Zhu, Xiancui; Li, Yang; Guo, Dianjun; Wang, Shaowu; Wei, Yun; Zhou, Shuangliu; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3947–3957; doi:10.1039/c7dt04410k

data_7045564
_publ_section_title
;
 Versatile reactivities of rare-earth metal dialkyl complexes supported by
 a neutral pyrrolyl-functionalized \b-diketiminato ligand.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3947
_journal_page_last               3957
_journal_paper_doi               10.1039/c7dt04410k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C83 H129 N9 S3 Si2 Y2'
_chemical_formula_sum            'C83 H129 N9 S3 Si2 Y2'
_chemical_formula_weight         1583.12
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.5309(16)
_cell_length_b                   13.4806(9)
_cell_length_c                   27.6008(18)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.20
_cell_volume                     9477.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_number            21515
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.7738
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.4988
_refine_diff_density_max         1.165
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         21515
_refine_ls_number_restraints     1997
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1115P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12858
_reflns_number_total             21515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04410k2.cif
_cod_data_source_block           8a
_cod_depositor_comments
'Adding full bibliography for 7045551--7045564.cif.'
_cod_database_code               7045564
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.746
_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
 H17A-H18B
 1.9 with sigma of 0.02
3. Rigid bond restraints
 Si1, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C53, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. 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 C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Si1 \\sim C27: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Si1 \\sim C28: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Si1 \\sim C29: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(Si1) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
5.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C36(H36), C43(H43), C61(H61), C68(H68)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C26(H26A,H26B), C30(H30A,H30B), C51(H51A,
 H51B), C52(H52A,H52B), C76(H76A,H76B), C77(H77A,H77B)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C22(H22), C23(H23), C38(H38), C39(H39),
 C40(H40), C48(H48), C55(H55), C56(H56), C63(H63), C64(H64), C65(H65), C80(H80),
  C81(H81)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C75(H75A,H75B,H75C), C78(H78A,H78B,H78C), C83(H83A,H83B,
 H83C)
;
_shelx_res_checksum              56023
_shelx_fab_checksum              33129
_olex2_submission_special_instructions 'No special instructions were received'