Rare earth metal bisamido complexes with a NNO tridentate ligand and catalytic activity for selective polymerization of isoprene
Gu, Xiaoxia; Wang, Shaowu; Wei, Yun; Zhu, Xiancui; Zhou, Shuangliu; Huang, Zeming; Mu, Xiaolong; New J. Chem. 41 (2017) 7723–7728; doi:10.1039/C7NJ01454F

data_7056358
_publ_section_title
;
 Rare earth metal bisamido complexes with a NNO tridentate ligand and
 catalytic activity for selective polymerization of isoprene
;
_journal_issue                   15
_journal_name_full               'New J. Chem.'
_journal_page_first              7723
_journal_page_last               7728
_journal_paper_doi               10.1039/C7NJ01454F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C24 H51 Gd N4 O Si4'
_chemical_formula_sum            'C24 H51 Gd N4 O Si4'
_chemical_formula_weight         681.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-17 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.2840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8027(16)
_cell_length_b                   12.4348(12)
_cell_length_c                   17.2821(16)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.47
_cell_volume                     3541.1(6)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30170
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.682
_diffrn_reflns_theta_min         1.638
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick,1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00266(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         8246
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.8161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6807
_reflns_number_total             8246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01454f2.cif
_cod_data_source_block           4_0m
_cod_database_code               7056358
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.699
_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
 C19-C20 \\sim C20-C21 \\sim C21-C19 \\sim C19'-C20' \\sim C20'-C21' \\sim
C21'-C19'
 with sigma of 0.02
 Si3-C19 \\sim Si3-C20 \\sim Si3-C21 \\sim Si3-C19' \\sim Si3-C20' \\sim
Si3-C21'
 with sigma of 0.02
3. Rigid bond restraints
 Si2, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si3, C19, C20, C21, C19', C20', C21'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Si2 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Si3 \\sim C19 \\sim C20 \\sim C21 \\sim C19' \\sim C20' \\sim C21': within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C19')=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20')=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C21'(H21D,H21E,H21F), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              17698
_olex2_submission_special_instructions 'No special instructions were received'