Synthesis of γ-amidine-functionalized dianionic β-diketiminato lanthanide amides and trianionic β-diketiminato Na/Sm heterobimetallic complexes and their reactivity in polymerization of l-lactide.
Liu, Peng; Chen, Hongxia; Zhang, Yong; Xue, Mingqiang; Yao, Yingming; Shen, Qi; Dalton transactions (Cambridge, England : 2003) 43 (2014) 5586–5594; doi:10.1039/c3dt52706a

data_7029364
_publ_section_title
;
 Synthesis of \g-amidine-functionalized dianionic \b-diketiminato
 lanthanide amides and trianionic \b-diketiminato Na/Sm heterobimetallic
 complexes and their reactivity in polymerization of l-lactide.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5586
_journal_page_last               5594
_journal_paper_doi               10.1039/c3dt52706a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C50 H91 N5 Na O4 Si2 Sm'
_chemical_formula_sum            'C50 H91 N5 Na O4 Si2 Sm'
_chemical_formula_weight         1055.80
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3799(10)
_cell_length_b                   23.828(2)
_cell_length_c                   39.619(3)
_cell_measurement_reflns_used    48823
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     11687.1(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            53353
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         10077
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.344
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.1198
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+57.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                8338
_reflns_number_total             10077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52706a.txt
_cod_data_source_block           complex5
_cod_original_cell_volume        11687.4(17)
_cod_database_code               7029364