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_4319113
_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            'C33 H30 Er N5 Se'
_chemical_formula_weight         742.84
_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                90.000(10)
_cell_angle_beta                 91.62(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   11.864(3)
_cell_length_b                   14.188(2)
_cell_length_c                   17.624(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      13.0
_cell_volume                     2965.4(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5119
_diffrn_reflns_theta_full        23.97
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_T_max  0.5996
_exptl_absorpt_correction_T_min  0.4478
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.914
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00219(17)
_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   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4639
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                4151
_reflns_number_total             4639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000499y_2.cif
_cod_data_source_block           erseazo
_cod_database_code               4319113