Syntheses, Structures, and Properties of the Bis(cyclopentadienyl) Rare-Earth Imidodiphosphinochalcogenido Compounds Cp2Ln[N(QPPh2)2] (Ln = La, Gd, Er, or Yb for Q = Se; Ln = Yb for Q = S)
Christopher G. Pernin; James A. Ibers; Inorganic Chemistry 39 (2000) 1216–1221; doi:10.1021/ic990889o

data_4300140
_publ_section_title
;
Syntheses, Structures, and Properties of the Bis(cyclopentadienyl)
Rare-Earth Imidodiphosphinochalcogenido Compounds Cp2Ln[N(QPPh2)2] (Ln =
La, Gd, Er, or Yb for Q = Se; Ln = Yb for Q = S)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1216
_journal_page_last               1221
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C34 H30 N P2 S2 Yb'
_chemical_formula_weight         751.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.102(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8799(18)
_cell_length_b                   12.6747(16)
_cell_length_c                   17.180(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      1.87
_cell_volume                     3021.8(7)
_computing_cell_refinement       'SAINT PLUS (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT PLUS (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD Diffractometer'
_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  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31187
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    3.364
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   'semi-empirical, ellipsoidal'
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1492
_refine_diff_density_max         2.672
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l] 
 where P = 1.00000Fo^2^ + 0.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                6698
_reflns_number_total             7286
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300140
_journal_paper_doi 10.1021/ic990889o