Relationship between the Skew Angle and Interplanar Distance in Four Bis(phthalocyaninato)lanthanide(III) Tetrabutylammonium Salts ([NBun4][LnIIIPc2]; Ln = Nd, Gd, Ho, Lu)
Naoto Koike; Hidehiro Uekusa; Yuji Ohashi; Chokto Harnoode; Fusao Kitamura; Takeo Ohsaka; Koichi Tokuda; Inorganic Chemistry 35 (1996) 5798–5804; doi:10.1021/ic960158d

data_4323904
_publ_section_title
;
 Relationship between the Skew Angle and Interplanar Distance in Four
 Bis(phthalocyaninato)lanthanide(III) Tetrabutylammonium Salts
 ([NBun4][LnIIIPc2]; Ln = Nd, Gd, Ho, Lu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5798
_journal_page_last               5804
_journal_paper_doi               10.1021/ic960158d
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C80 H68 Gd N17'
_chemical_formula_weight         1424.76
_chemical_name_systematic
; 
tetrabutylammonium bis(phtahlocyaninato)-gadolinium(iii)  
;
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.399(8)
_cell_length_b                   17.399
_cell_length_c                   11.377(6)
_cell_measurement_temperature    296(2)
_cell_volume                     3444(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SAPI-91 (Fan Hai-Fu, 1991)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device
;Rigaku Catg, R-Axis IIcs, Weissenberg type diffractometer diffractometer
with Imaging plates
;
_diffrn_measurement_method       'Imaging plate'
_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  0.2191
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3284
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_type   n
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             1462
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         .729
_refine_diff_density_min         -.513
_refine_diff_density_rms         .079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.123
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_obs          0.0782
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1276P)^2^+3.9707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2531
_refine_ls_wR_factor_obs         0.2124
_reflns_number_observed          1932
_reflns_number_total             2932
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960158d_2.cif
_cod_data_source_block           gdpc2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1276P)^2^+3.9707P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.1276P)^2^+3.9707P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3444.1(23)
_cod_database_code               4323904