Half-Sandwich Rare-Earth Metal Complexes Bearing a C5Me4-C6H4-o-CH2NMe2 Ligand: Synthesis, Characterization and Catalytic Properties for Isoprene, 1-Hexene and MMA Polymerization
Mu, Ying; Song, Tingting; Liu, Ning; Tong, Xiaobo; Li, Feng; Mu, Xiaoyue; Dalton Transactions  (2019) –; doi:10.1039/C9DT04029C

data_7701988
_publ_section_title
;
 Half-Sandwich Rare-Earth Metal Complexes Bearing a C5Me4-C6H4-o-CH2NMe2
 Ligand: Synthesis, Characterization and Catalytic Properties for
 Isoprene, 1-Hexene and MMA Polymerization
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT04029C
_journal_year                    2019
_chemical_formula_moiety         'C36 H58 B4 N2 Sm2'
_chemical_formula_sum            'C36 H64 B4 N2 Sm2'
_chemical_formula_weight         868.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.1500(10)
_cell_angle_beta                 94.7390(10)
_cell_angle_gamma                96.5830(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6992(5)
_cell_length_b                   12.4170(7)
_cell_length_c                   21.8057(12)
_cell_measurement_reflns_used    7838
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.37
_cell_volume                     2329.3(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.966
_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  0.0186
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13240
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.377
_diffrn_reflns_theta_min         2.366
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         9200
_refine_ls_number_restraints     945
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0597P)^2^+4.2148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7998
_reflns_number_total             9200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04029c2.cif
_cod_data_source_block           2_sq_sq
_cod_database_code               7701988
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.646
_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. Rigid bond restraints
 C19, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Sm1, B2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Sm2, B2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C26 \\sim C25 \\sim C27 \\sim C6 \\sim C1 \\sim C11 \\sim C29 \\sim C7 \\sim C5
\\sim C3 \\sim C28 \\sim C4 \\sim C33 \\sim C12 \\sim C19 \\sim C24 \\sim C30
\\sim C31 \\sim C22 \\sim C16 \\sim C23 \\sim C32 \\sim C8 \\sim C17 \\sim C20
\\sim C21 \\sim C18 \\sim C15 \\sim C36 \\sim C35 \\sim C34 \\sim C10 \\sim C9
\\sim C2 \\sim C14 \\sim C13: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C34(H34A,H34B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C22(H22), C23(H23), C20(H20), C21(H21), C2(H2)
4.c Idealised Me refined as rotating group:
 C33(H33C,H33A,H33B), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C15(H15A,
 H15B,H15C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              34599
_shelx_fab_checksum              175
_olex2_submission_special_instructions 'No special instructions were received'