Soluble Yttrium Chalcogenides: Syntheses, Structures, and NMR Properties of Y[η3-N(SPPh2)2]3 and Y[η2-N(SePPh2)2]2[η3-N(SePPh2)2]
Christopher G. Pernin; James A. Ibers; Inorganic Chemistry 39 (2000) 1222–1226; doi:10.1021/ic990984x

data_4300152
_publ_section_title
;
Soluble Yttrium Chalcogenides: Syntheses, Structures, and NMR Properties
of Y[\h3-N(SPPh2)2]3 and Y[\h2-N(SePPh2)2]2[\h3-N(SePPh2)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1222
_journal_page_last               1226
_journal_paper_doi               10.1021/ic990984x
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C72 H60 N3 P6 S6 Y'
_chemical_formula_weight         1434.32
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.927(5)
_cell_length_b                   14.927(5)
_cell_length_c                   56.047(13)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    153(2)
_cell_volume                     10815(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            17809
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <2%
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   'numerical, face-indexed'
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4428
_exptl_crystal_size_max          0.20mm
_exptl_crystal_size_min          0.09mm
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.0797
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                1451
_reflns_number_total             2128
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4300152