Selective ammonolysis of half-sandwich rare-earth metal dialkyl and polyhydride complexes: synthesis of polyamido rare-earth complexes having novel structures.
Shima, Takanori; Hou, Zhaomin; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6858–6863; doi:10.1039/c0dt00006j

data_7025801
_publ_section_title
;
 Selective ammonolysis of half-sandwich rare-earth metal dialkyl and
 polyhydride complexes: synthesis of polyamido rare-earth complexes having
 novel structures.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6858
_journal_page_last               6863
_journal_paper_doi               10.1039/c0dt00006j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C36 H75 N6 Sc3 Si3'
_chemical_formula_weight         811.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                94.484(3)
_cell_angle_beta                 103.470(3)
_cell_angle_gamma                104.442(3)
_cell_formula_units_Z            2
_cell_length_a                   12.587(2)
_cell_length_b                   13.134(2)
_cell_length_c                   14.841(3)
_cell_measurement_reflns_used    15170
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.43
_cell_volume                     2286.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_sigmaI/netI    0.1553
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15170
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.8545
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.155
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         9934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1139P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2347
_reflns_number_gt                5660
_reflns_number_total             9934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00006j.txt
_cod_data_source_block           3Sc
_cod_original_cell_volume        2286.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025801