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_7045553
_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         'C74 H104 Er2 N6 Si2'
_chemical_formula_sum            'C74 H104 Er2 N6 Si2'
_chemical_formula_weight         1468.33
_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   geom
_audit_creation_date             2018-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-05 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                88.1770(10)
_cell_angle_beta                 68.3690(10)
_cell_angle_gamma                76.2840(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8774(14)
_cell_length_b                   13.9863(17)
_cell_length_c                   15.4143(19)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.65
_cell_volume                     2308.0(5)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            8088
_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         1.424
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  0.6954
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.4890
_refine_diff_density_max         1.379
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8088
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0644P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5837
_reflns_number_total             8088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04410k2.cif
_cod_data_source_block           5c
_cod_depositor_comments
'Adding full bibliography for 7045551--7045564.cif.'
_cod_database_code               7045553
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.695
_shelx_estimated_absorpt_t_min   0.674
_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
 C2-C3
 1.5 with sigma of 0.02
 C1-C3
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C24 \\sim C23 \\sim C22 \\sim C21 \\sim C25 \\sim C20 \\sim C19 \\sim C18 \\sim
C17 \\sim C16 \\sim C15 \\sim C13 \\sim C14 \\sim C9 \\sim C4 \\sim C5 \\sim C6
\\sim C7 \\sim C8 \\sim C3 \\sim C1 \\sim C2 \\sim C10 \\sim C12 \\sim C11
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
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
Uanis(C3) \\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)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C15(H15), C5(H5), C6(H6), C7(H7), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37)
5.d Fitted hexagon refined as free rotating group:
 C32(C33,C34,C35,C36,C37)
5.e Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C14(H14A,H14B,
 H14C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              30819
_shelx_fab_checksum              49604
_olex2_submission_special_instructions 'No special instructions were received'