Strategies for the Synthesis of Lanthanum Dialkyl Complexes with Monoanionic Ancillary Ligands
Bambirra, Sergio; Perazzolo, Francesca; Boot, Steven J.; Sciarone, Timo J. J.; Meetsma, Auke; Hessen, Bart; Organometallics 27 (2008) 704–; doi:10.1021/om700919h

data_4070667
_publ_section_title
;
 Strategies for the Synthesis of Lanthanum Dialkyl Complexes with
 Monoanionic Ancillary Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              704
_journal_paper_doi               10.1021/om700919h
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         '2(C28 H47 La N4 Si), C6 H6'
_chemical_formula_sum            'C62 H100 La2 N8 Si2'
_chemical_formula_weight         1291.51
_chemical_name_systematic        ?
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2006-05-17  08:36:02'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version ::  40506)
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
 ?
;
_cell_angle_alpha                90
_cell_angle_beta                 94.561(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.277(1)
_cell_length_b                   9.7710(6)
_cell_length_c                   18.618(1)
_cell_measurement_reflns_used    6564
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.36
_cell_volume                     3133.0(3)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2006)
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25838
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_T_max  0.8707
_exptl_absorpt_correction_T_min  0.7030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
  Enantiomorph twin refinement resulted in 0.522(9) 
   Flack, H.D. & Bernardinelli, G. (1999, 2000)
;
_refine_ls_abs_structure_Flack   0.522(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         12652
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+1.3003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                12294
_reflns_number_total             12652
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om700919h-file003.cif
_cod_data_source_block           Q1111
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4070667
_vrn_publ_code_void_volume       23.6
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    9.2