Chiral bis(phthalocyaninato) yttrium double-decker complexes. Synthesis, structure, spectroscopy, and electrochemistry.
Zhou, Hang; Wang, Kang; Qi, Dongdong; Jiang, Jianzhuang; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1699–1705; doi:10.1039/c3dt52611a

data_7028328
_publ_section_title
;
 Chiral bis(phthalocyaninato) yttrium double-decker complexes. Synthesis,
 structure, spectroscopy, and electrochemistry.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1699
_journal_page_last               1705
_journal_paper_doi               10.1039/c3dt52611a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C224 H112 N16 O16 Y'
_chemical_formula_weight         3372.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.5507(5)
_cell_length_b                   21.5507(5)
_cell_length_c                   22.5192(14)
_cell_measurement_reflns_used    2978
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      63.7715
_cell_measurement_theta_min      3.4991
_cell_volume                     10458.7(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 16.2141
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8391
_diffrn_reflns_theta_full        63.87
_diffrn_reflns_theta_max         63.87
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.8433
_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_colour            green
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3470
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
In this compound, the unit cell includes a large region of disordered 
solvent molecules, which could not be modeled as discrete atomic sites. 
We employed PLATON/SQUEEZE to calculate the diffraction contribution 
of the solvent molecules and, thereby, to produce a set of solvent-free 
diffraction intensities. The SQUEEZE calculations showed a total solvent 
accessible area volume of 1731 A^3^ in this compound and the residual 
electron density amounted to 481 electron per unit cell, corresponding to 
nearly 8 molecules of CH2Cl2 and 8 molecules of CH3OH 
(about 2 CH2Cl2 and 2 CH3OH molecules per asymmetric unit).
;
_refine_diff_density_max         2.212
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.057(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         5923
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1018P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                5368
_reflns_number_total             5923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52611a.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7028328