Anhydrous Lanthanide Schiff Base Complexes and Their Preparation Using Lanthanide Triflate Derived Amides
Steven A. Schuetz; Victor W. Day; Roger D. Sommer; Arnold L. Rheingold; John A. Belot; Inorganic Chemistry 40 (2001) 5292–5295; doi:10.1021/ic010060l

data_4320281
_publ_contact_author
;
  Professor John Belot
  University of Nebraska-Lincoln
  746 Hamilton Hall
  Lincoln, NE-68588-0304
;
_publ_contact_author_email       jbelot2@unl.edu
_publ_section_title
;
 Anhydrous Lanthanide Schiff Base Complexes and Their Preparation Using
 Lanthanide Triflate Derived Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5292
_journal_page_last               5295
_journal_paper_doi               10.1021/ic010060l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C25 H50 N3 O2 Si2 Sm'
_chemical_formula_weight         631.21
_chemical_melting_point          407.35
_chemical_name_systematic
;
  Bis-5,5'-(1,3-propanediyldiimino)-2,2-dimethyl-4-hexene-3-onato 
samarium bis(trimethylsilyl)-amido
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.338(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6401(15)
_cell_length_b                   25.826(4)
_cell_length_c                   12.042(2)
_cell_measurement_reflns_used    918
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      55.59
_cell_measurement_theta_min      5.51
_cell_volume                     3175.4(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Bruker SMART CCD Area Detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20423
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.6884
_exptl_absorpt_correction_T_min  0.5724
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       'Irregular chunk'
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.939
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.939
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_obs          0.0327
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0616
_refine_ls_wR_factor_obs         0.0562
_reflns_number_observed          5446
_reflns_number_total             7581
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010060l_1.cif
_cod_data_source_block           jbb3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320281