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_7701985
_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 H64 B4 N2 Nd2'
_chemical_formula_sum            'C36 H64 B4 N2 Nd2'
_chemical_formula_weight         856.61
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-23 deposited with the CCDC.	2019-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.094(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.732(6)
_cell_length_b                   22.278(14)
_cell_length_c                   24.533(16)
_cell_measurement_reflns_used    5015
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.48
_cell_volume                     4712(5)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26636
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         1.681
_exptl_absorpt_coefficient_mu    2.200
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         9621
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8137
_reflns_number_total             9621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04029c2.cif
_cod_data_source_block           1_sq
_cod_database_code               7701985
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.632
_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
 B3-H3B
 1.1 with sigma of 0.02
 B3-H3D
 1.1 with sigma of 0.02
 B3-H3A
 1.1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C20(H20), C4(H4), C23(H23), C3(H3), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C13(H13A,
 H13B,H13C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              32917
_shelx_fab_checksum              43111
_olex2_submission_special_instructions 'No special instructions were received'