Heteroleptic Tm(II) Complexes: One More Success for Trofimenko's Scorpionates
Jianhua Cheng; Josef Takats; Michael J. Ferguson; Robert McDonald; Journal of the American Chemical Society 130 (2008) 1544–1545; doi:10.1021/ja0776273

data_4107377
_publ_section_title
;
 Heteroleptic Tm(II) Complexes: One More Success for Trofimenko's
 Scorpionates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1544
_journal_page_last               1545
_journal_paper_doi               10.1021/ja0776273
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C76 H124 B2 N16 Tm2, C6 H14'
_chemical_formula_sum            'C82 H138 B2 N16 Tm2'
_chemical_formula_weight         1707.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4127(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.598(3)
_cell_length_b                   15.571(2)
_cell_length_c                   24.217(3)
_cell_measurement_reflns_used    7675
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.64
_cell_measurement_theta_min      2.28
_cell_volume                     8895.7(19)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w 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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39202
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.030
_exptl_absorpt_correction_T_max  0.7927
_exptl_absorpt_correction_T_min  0.3960
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 Attempts to refine peaks of residual electron density as solvent n-hexane
 carbon atoms were unsuccessful.  The data were corrected for disordered
 electron density through use of the SQUEEZE procedure (Sluis, P. van der;
 Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON
 (Spek, A.L. Acta Crystallogr. 1990, A46, C34.  PLATON - a multipurpose
 crystallographic tool.  Utrecht University, Utrecht, The Netherlands).
 A total solvent-accessible void volume of 1215.9 A^3^ with a total
 electron count of 210 (consistent with four molecules of solvent n-hexane,
 or one molecule per formula unit of the dithulium complex molecule) was
 found in the unit cell.
;
_refine_diff_density_max         7.436
_refine_diff_density_min         -3.004
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.085(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         20302
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0548P)^2^+137.7370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                19458
_reflns_number_total             20302
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0776273-file003_6.cif
_cod_data_source_block           6
_cod_original_cell_volume        8896(2)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4107377