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_7045562
_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         'C38.04 H63.12 Er N4 Si2'
_chemical_formula_sum            'C38.04 H63.11 Er N4 Si2'
_chemical_formula_weight         799.93
_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
_audit_creation_date             2018-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-30 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6567(8)
_cell_length_b                   19.5163(13)
_cell_length_c                   18.9209(13)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.22
_cell_volume                     4277.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      293.15
_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  0.0322
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32065
_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         25.371
_diffrn_reflns_theta_min         1.504
_exptl_absorpt_coefficient_mu    2.046
_exptl_absorpt_correction_T_max  0.6851
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             1661
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.5304
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7835
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0337P)^2^+2.1272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6459
_reflns_number_total             7835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04410k2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7045551--7045564.cif.'
_cod_database_code               7045562
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1A-C26 \\sim Si1B-C26
 with sigma of 0.02
 Si1A-C28B \\sim Si1A-C29A \\sim Si1B-C29B \\sim Si1B-C28 \\sim Si1B-C27A \\sim
Si1A-C27B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si1A) = Uanis(Si1B)
4. Others
 Sof(Si1A)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(Si1B)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
 Fixed Sof: H26B(0.67) H26A(0.67) H26D(0.33) H26C(0.33) C27B(0.33) H27A(0.33)
 H27B(0.33) H27C(0.33) C28(0.67) H28A(0.67) H28B(0.67) H28C(0.67) C29B(0.67)
 H29A(0.67) H29B(0.67) H29C(0.67)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C11(H11)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C26(H26B,H26A), C26(H26D,H26C), C30(H30A,H30B)
5.c Me refined with riding coordinates:
 C27B(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29B(H29A,H29B,H29C), C28B(H28D,
 H28E,H28F), C27A(H27D,H27E,H27F), C29A(H29D,H29E,H29F)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C22(H22), C23(H23), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              65834
_olex2_submission_special_instructions 'No special instructions were received'