Mixed (Phthalocyaninato)(Porphyrinato) Rare Earth Double-Decker Complexes with C4 Chirality: Synthesis, Resolution, and Absolute Configuration Assignment
Yang Zhou; Yuexing Zhang; Hailong Wang; Jianzhuang Jiang; Yongzhong Bian; Atsuya Muranaka; Nagao Kobayashi; Inorganic Chemistry 48 (2009) 8925–8933; doi:10.1021/ic9011795

data_4303199
_publ_section_title
;
Mixed (Phthalocyaninato)(Porphyrinato) Rare Earth Double-Decker Complexes
with C4 Chirality: Synthesis, Resolution, and Absolute Configuration
Assignment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8925
_journal_page_last               8933
_journal_paper_doi               10.1021/ic9011795
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C128 H152 N16 O4 Y'
_chemical_formula_weight         2067.57
_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                96.307(2)
_cell_angle_beta                 103.4020(10)
_cell_angle_gamma                112.204(2)
_cell_formula_units_Z            2
_cell_length_a                   13.784(3)
_cell_length_b                   16.728(3)
_cell_length_c                   27.926(6)
_cell_measurement_temperature    293(2)
_cell_volume                     5658(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.2078
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28398
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.9393
_exptl_absorpt_correction_T_min  0.9236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            collourless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2206
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         19780
_refine_ls_number_restraints     4585
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2472
_refine_ls_R_factor_gt           0.1070
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2750
_refine_ls_wR_factor_ref         0.3760
_reflns_number_gt                7539
_reflns_number_total             19780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9011795_si_001.cif
_cod_data_source_block           qq
_cod_original_cell_volume        5658.3(19)
_cod_database_code               4303199