Amido-stabilized rare-earth metal mixed methyl methylidene complexes
Zimmermann, Melanie; Rauschmaier, Dorothea; Eichele, Klaus; Törnroos, Karl W.; Anwander, Reiner; Chemical Communications 46 (2010) 5346–5348; doi:10.1039/c003206a

data_7111628
_publ_section_title
;
 Amido-stabilized rare-earth metal mixed methyl methylidene complexes
;
_journal_issue                   29
_journal_name_full               'Chemical Communications'
_journal_page_first              5346
_journal_page_last               5348
_journal_paper_doi               10.1039/c003206a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C62 H116 Lu3 N3 O3 Si3, 2(C4 H8 O)'
_chemical_formula_sum            'C70 H132 Lu3 N3 O5 Si3'
_chemical_formula_weight         1704.97
_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                99.559(1)
_cell_angle_beta                 96.973(1)
_cell_angle_gamma                105.926(1)
_cell_formula_units_Z            2
_cell_length_a                   11.6347(7)
_cell_length_b                   13.0521(8)
_cell_length_c                   28.3440(16)
_cell_measurement_reflns_used    19596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.48
_cell_volume                     4017.8(4)
_computing_cell_refinement
;
Bruker (2008). SAINT, version 6.45A, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_molecular_graphics
;
Brandenburg, K. (2007). DIAMOND. Version 3.1. Crystal Impact GbR, Bonn,
Germany.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_computing_structure_solution
;
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'TXS Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            47500
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    3.745
_exptl_absorpt_correction_T_max  0.4545
_exptl_absorpt_correction_T_min  0.2835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS version 2008/1, G.M Sheldrick, University of
G\"ttingen, Germany, 2008.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         5.026
_refine_diff_density_min         -6.160
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         23137
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0001P)^2^+38.7001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                19572
_reflns_number_total             23137
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C003206Asup1.cif
_cod_data_source_block           zm118
_cod_database_code               7111628