Sandwich-Type Mixed Tetrapyrrole Rare-Earth Triple-Decker Compounds. Effect of the Coordination Geometry on the Single-Molecule-Magnet Nature
Jinglan Kan; Hailong Wang; Wei Sun; Wei Cao; Jun Tao; Jianzhuang Jiang; Inorganic Chemistry 52 (2013) 8505–8510; doi:10.1021/ic400485y

data_4335536
_publ_contact_author_address
; 
Department of Chemistry, University of
 Science and Technology Beijing, Beijing 
100083, China 
;
_publ_contact_author_email       kanjinglan@163.com
_publ_contact_author_name        'Jianzhuang Jiang'
_publ_section_title
;
 Sandwich-Type Mixed Tetrapyrrole Rare-Earth Triple-Decker Compounds.
 Effect of the Coordination Geometry on the Single-Molecule-Magnet Nature
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8505
_journal_page_last               8510
_journal_paper_doi               10.1021/ic400485y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C212 H136 Cl28 Dy N20 O20 Y'
_chemical_formula_weight         4527.32
_chemical_name_systematic
; 
 ? 
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_cell_measurement_reflns_used    22357
_cell_measurement_temperature    107(20)
_cell_measurement_theta_max      63.9716
_cell_measurement_theta_min      3.0343
_cell_volume                     10808.47(19)
_computing_cell_refinement
;CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;   
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      107(20)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46950
_diffrn_reflns_theta_full        63.91
_diffrn_reflns_theta_max         63.91
_diffrn_reflns_theta_min         3.04
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.910
_exptl_absorpt_correction_T_max  0.6492
_exptl_absorpt_correction_T_min  0.4709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.  
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             4554
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.514
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_coef       0.00098(9)
_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   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8841
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0808
_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 w=1/[\s^2^(Fo^2^)+(0.1582P)^2^+14.9073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2269
_reflns_number_gt                7875
_reflns_number_total             8841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400485y_si_002_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     'P4-2n '
_cod_database_code               4335536