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_7029362
_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         'C48 H80 N5 Si2 Y'
_chemical_formula_sum            'C48 H80 N5 Si2 Y'
_chemical_formula_weight         872.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.532(6)
_cell_angle_beta                 82.510(5)
_cell_angle_gamma                87.367(6)
_cell_formula_units_Z            2
_cell_length_a                   11.4805(7)
_cell_length_b                   12.4211(12)
_cell_length_c                   17.5400(9)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.4327
_cell_measurement_theta_min      3.2905
_cell_volume                     2467.2(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_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      200(2)
_diffrn_detector_area_resol_mean 10.4692
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22943
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9141
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                7407
_reflns_number_total             9141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52706a.txt
_cod_data_source_block           complex3
_cod_database_code               7029362