Heteroleptic Lanthanide Compounds with Chalcogenolate Ligands: Reduction of PhNNPh/PhEEPh (E = Se or Te) Mixtures with Ln (Ln = Ho, Er, Tm, Yb). Thermolysis Can Give LnN or LnE
Anna Kornienko; Deborah Freedman; Thomas J. Emge; John G. Brennan; Inorganic Chemistry 40 (2001) 140–145; doi:10.1021/ic000499y

data_4319112
_publ_contact_author_address
; 
 Department of Chemistry 
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey  08854-8087  U.S.A. 
;
_publ_contact_author_email       bren@rutchem.rutgers.edu
_publ_contact_author_name        'J. G. Brennan'
_publ_section_title
;
 Heteroleptic Lanthanide Compounds with Chalcogenolate Ligands: Reduction
 of PhNNPh/PhEEPh (E = Se or Te) Mixtures with Ln (Ln = Ho, Er, Tm, Yb).
 Thermolysis Can Give LnN or LnE
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              140
_journal_page_last               145
_journal_paper_doi               10.1021/ic000499y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C66 H60 Ho2 N10 Te2'
_chemical_formula_weight         1578.30
_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                75.82(3)
_cell_angle_beta                 74.11(3)
_cell_angle_gamma                89.45(2)
_cell_formula_units_Z            2
_cell_length_a                   10.349(2)
_cell_length_b                   17.662(4)
_cell_length_c                   17.730(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      15.3
_cell_measurement_theta_min      14.1
_cell_volume                     3016.2(18)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'local program'
_computing_molecular_graphics    'XPMA/ZORTEP (Zsolnai, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(5)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius CAD4 diffractometer'
_diffrn_measurement_method       'omega-theta scans'
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10014
_diffrn_reflns_theta_full        23.99
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.8729
_exptl_absorpt_correction_T_min  0.7273
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.950
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00004(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     1332
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                7040
_reflns_number_total             9411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000499y_1.cif
_cod_data_source_block           hoteazo
_cod_original_cell_volume        3016.2(16)
_cod_database_code               4319112