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_7045563
_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         'C37 H66 Er N3 O Si2'
_chemical_formula_sum            'C37 H66 Er N3 O Si2'
_chemical_formula_weight         792.36
_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             2018-01-29
_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                 116.3480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3174(16)
_cell_length_b                   19.3447(13)
_cell_length_c                   21.0762(14)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.20
_cell_volume                     8519.2(10)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.434
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  0.7761
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         16729
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+2.0601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10323
_reflns_number_total             16729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04410k2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7045551--7045564.cif.'
_cod_database_code               7045563
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.709
_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
 C67-Si4 \\sim C67'-Si4'
 with sigma of 0.02
 Si4-C68 \\sim Si4-C69 \\sim Si4-C70 \\sim Si4'-C68' \\sim Si4'-C69' \\sim
Si4'-C70'
 with sigma of 0.02
 C68'-C69' \\sim C69'-C70' \\sim C70'-C68'
 with sigma of 0.02
 C68-C69 \\sim C69-C70 \\sim C70-C68
 with sigma of 0.02
 C34-C35 \\sim C34-C35'
 with sigma of 0.02
 C35-C36 \\sim C35'-C36'
 with sigma of 0.02
 C36-C37 \\sim C36'-C37
 with sigma of 0.02
 C71-C72 \\sim C71-C72'
 with sigma of 0.02
 C72-C73 \\sim C72'-C73'
 with sigma of 0.02
 C73-C74 \\sim C73'-C74
 with sigma of 0.02
3. Rigid bond restraints
 C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C68, C69, C70, C68', C69', C70'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si4, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si4, C68'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C68 \\sim C69 \\sim C70 \\sim C68' \\sim C69' \\sim C70': within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C67')=Sof(H67C)=Sof(H67D)=
 Sof(C69')=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70')=Sof(H70D)=Sof(H70E)=
 Sof(H70F)=Sof(Si4')=1-FVAR(1)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=
 Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C68')=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(Si4)=
 FVAR(1)
 Fixed Sof: H34A(0.5) H34B(0.5) H34C(0.5) H34D(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5) C35'(0.5) H35C(0.5) H35D(0.5) C36'(0.5)
 H36C(0.5) H36D(0.5) H37A(0.5) H37B(0.5) H37C(0.5) H37D(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H71D(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5) H73A(0.5)
 H73B(0.5) C72'(0.5) H72C(0.5) H72D(0.5) C73'(0.5) H73C(0.5) H73D(0.5)
 H74A(0.5) H74B(0.5) H74C(0.5) H74D(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C39(H39), C47(H47)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C26(H26A,H26B), C30(H30A,H30B), C34(H34A,
 H34B), C34(H34C,H34D), C35(H35A,H35B), C36(H36A,H36B), C35'(H35C,H35D),
 C36'(H36C,H36D), C37(H37A,H37B), C37(H37C,H37D), C55(H55A,H55B), C56(H56A,
 H56B), C63(H63A,H63B), C67(H67A,H67B), C67'(H67C,H67D), C71(H71A,H71B),
 C71(H71C,H71D), C72(H72A,H72B), C73(H73A,H73B), C72'(H72C,H72D), C73'(H73C,
 H73D), C74(H74A,H74B), C74(H74C,H74D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C22(H22), C23(H23), C42(H42), C43(H43),
 C44(H44), C52(H52), C59(H59), C60(H60)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), 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), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C54(H54A,H54B,H54C), C57(H57A,H57B,H57C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C68'(H68D,H68E,H68F), C69'(H69D,H69E,
 H69F), C70'(H70D,H70E,H70F)
;
_shelx_res_checksum              51944
_olex2_submission_special_instructions 'No special instructions were received'