Constructing Sandwich-Type Rare Earth Double-Decker Complexes with N-Confused Porphyrinato and Phthalocyaninato Ligands
Wei Cao; Hailong Wang; Xin Wang; Hung Kay Lee; Dennis K. P. Ng; Jianzhuang Jiang; Inorganic Chemistry 51 (2012) 9265–9272; doi:10.1021/ic300789j

data_4330154
_publ_contact_author_address
; 
Department of Chemistry, University of
 Science and Technology Beijing, Beijing 
100083, China 
;
_publ_contact_author_name        'Jianzhuang Jiang'
_publ_section_title
;
 Constructing Sandwich-Type Rare Earth Double-Decker Complexes with
 N-Confused Porphyrinato and Phthalocyaninato Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9265
_journal_page_last               9272
_journal_paper_doi               10.1021/ic300789j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C96 H82 Cl9 N12 Y'
_chemical_formula_weight         1811.70
_chemical_name_systematic
; 
 ? 
;
_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                90.00
_cell_angle_beta                 99.164(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.0176(7)
_cell_length_b                   17.3764(5)
_cell_length_c                   36.3930(8)
_cell_measurement_reflns_used    12353
_cell_measurement_temperature    120
_cell_measurement_theta_max      65.2995
_cell_measurement_theta_min      3.1369
_cell_volume                     17491.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            57366
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    3.898
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             7472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2195
_refine_ls_number_reflns         29431
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1899P)^2^+5.8049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.2988
_reflns_number_gt                20051
_reflns_number_total             29431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300789j_si_002_1.cif
_cod_data_source_block           4
_cod_database_code               4330154