Anti-Bimetallic Complexes of Divalent Lanthanides with Silylated Pentalene and Cyclooctatetraenyl Bridging Ligands as Molecular Models for Lanthanide-Based Polymers
Summerscales, Owen T.; Jones, Simon C.; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Organometallics 28 (2009) 5896–; doi:10.1021/om900520h

data_4069938
_publ_section_title
;
 Anti-Bimetallic Complexes of Divalent Lanthanides with Silylated
 Pentalene and Cyclooctatetraenyl Bridging Ligands as Molecular Models for
 Lanthanide-Based Polymers
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5896
_journal_paper_doi               10.1021/om900520h
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H94 O2 Si2 Sm2, C6 H14'
_chemical_formula_sum            'C60 H108 O2 Si2 Sm2'
_chemical_formula_weight         1218.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-06-03T11:56:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.106(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9282(3)
_cell_length_b                   14.3909(5)
_cell_length_c                   18.0915(5)
_cell_measurement_reflns_used    62399
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3360.95(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.491013E-1
_diffrn_orient_matrix_UB_12      0.434815E-1
_diffrn_orient_matrix_UB_13      -0.270302E-1
_diffrn_orient_matrix_UB_21      0.225984E-1
_diffrn_orient_matrix_UB_22      0.512674E-1
_diffrn_orient_matrix_UB_23      0.345232E-1
_diffrn_orient_matrix_UB_31      0.554894E-1
_diffrn_orient_matrix_UB_32      0.175968E-1
_diffrn_orient_matrix_UB_33      -0.337904E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51794
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.8
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_correction_T_min  0.7779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.1
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         13142
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.092
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+2.1488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                9436
_reflns_number_total             13142
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900520h_si_004.cif
_cod_data_source_block           jun505
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4069938