A Novel Bis(imino)amine Ligand as a Result of Acetonitrile Coupling with the Diiodides of Dy(II) and Tm(II)
Mikhail N. Bochkarev; Georgii V. Khoroshenkov; Herbert Schumann; Sebastian Dechert; Journal of the American Chemical Society 125 (2003) 2894–2895; doi:10.1021/ja028311s

data_4113526
_publ_contact_author_address
; Razuvaev Institute of Organometallic Chemistry 
  Russian Academy of Sciences 
  Tropinina 49  
  603950 Nizhny Novgorod
  Russia 
;
_publ_contact_author_email       mboch@imoc.sinn.ru
_publ_contact_author_fax         (8312)66-67-95
_publ_contact_author_name        'Prof. Dr. M. N. Bochkarev'
_publ_contact_author_phone       (8312)66-14-97
_publ_section_title
;
 A Novel Bis(imino)amine Ligand as a Result of Acetonitrile Coupling with
 the Diiodides of Dy(II) and Tm(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2894
_journal_page_last               2895
_journal_paper_doi               10.1021/ja028311s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C18 H31 N9 Tm 3+, 3 I 1-, 2(C2 H3 N)'
_chemical_formula_sum            'C22 H37 I3 N11 Tm'
_chemical_formula_weight         1005.26
_chemical_name_systematic
; 
 ? 
;
_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                69.641(1)
_cell_angle_beta                 89.732(1)
_cell_angle_gamma                73.989(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7188(3)
_cell_length_b                   13.7619(5)
_cell_length_c                   14.0021(5)
_cell_measurement_reflns_used    3647
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      1.56
_cell_volume                     1851.75(11)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, Pritzkow, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12405
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_T_max  0.694916
_exptl_absorpt_correction_T_min  0.437734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7169
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                5054
_reflns_number_total             7169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028311ssi20021230_025705_1.cif
_cod_data_source_block           Ic
_cod_database_code               4113526