Synthesis and Structural Characterization of Sm(II) and Yb(II) Complexes Containing Sterically Demanding, Chelating Secondary Phosphide Ligands
Keith Izod; Paul O'Shaughnessy; Joanne M. Sheffield; William Clegg; Stephen T. Liddle; Inorganic Chemistry 39 (2000) 4741–4748; doi:10.1021/ic0002871

data_4321452
_publ_section_title
;
 Synthesis and Structural Characterization of Sm(II) and Yb(II) Complexes
 Containing Sterically Demanding, Chelating Secondary Phosphide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4741
_journal_page_last               4748
_journal_paper_doi               10.1021/ic0002871
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C38 H76 O5 P2 Si4 Sm'
_chemical_formula_weight         937.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.363(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.176(4)
_cell_length_b                   13.080(4)
_cell_length_c                   14.546(4)
_cell_measurement_reflns_used    10266
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.11
_cell_volume                     2495.9(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1378
_diffrn_reflns_av_sigmaI/netI    0.2061
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13180
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.803
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.24(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7193
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2533
_reflns_number_gt                4695
_reflns_number_total             7193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002871_2.cif
_cod_data_source_block           ki31
_cod_database_code               4321452