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_4300137
_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 Gd N P2 Se2'
_chemical_formula_weight         829.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.062(2)
_cell_angle_beta                 87.613(2)
_cell_angle_gamma                69.041(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7130(14)
_cell_length_b                   12.2659(17)
_cell_length_c                   13.953(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    153(2)
_cell_volume                     1550.7(4)
_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 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13055
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    4.613
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   'numerical, face-indexed'
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.732
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.732
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_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          0.0632
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                5064
_reflns_number_total             7056
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4300137
_journal_paper_doi 10.1021/ic990889o