α-Substituted Bis(octabutoxyphthalocyaninato)Terbium(III) Double-Decker Complexes: Preparation and Study of Protonation by NMR and DFT.
Damjanović, Marko; Horie, Yusuke; Morita, Takaumi; Horii, Yoji; Katoh, Keiichi; Yamashita, Masahiro; Enders, Markus; Inorganic chemistry 54 (2015) 11986–11992; doi:10.1021/acs.inorgchem.5b02391

data_4346942
_publ_section_title
;
 \a-Substituted Bis(octabutoxyphthalocyaninato)Terbium(III) Double-Decker
 Complexes: Preparation and Study of Protonation by NMR and DFT.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11986
_journal_page_last               11992
_journal_paper_doi               10.1021/acs.inorgchem.5b02391
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C128 H160 N16 O16 Tb'
_chemical_formula_weight         2337.64
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.1330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.247(3)
_cell_length_b                   21.5720(17)
_cell_length_c                   17.6315(14)
_cell_measurement_reflns_used    26760
_cell_measurement_temperature    90
_cell_measurement_theta_max      0.933
_cell_measurement_theta_min      0.892
_cell_volume                     11699.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\f and \w scan'
_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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            100180
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4932
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1467
_refine_ls_number_reflns         26760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0444P)^2^+31.2716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                17877
_reflns_number_total             26760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02391_si_002.cif
_cod_data_source_block           20150312_outa_a
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 

The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        11699.5(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4346942