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_4323906
_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 H70 Lu N17 O'
_chemical_formula_weight         1460.50
_chemical_name_systematic
; 
tetrabutylammonium bis(phtahlocyaninato)-lutetium(iii) water solvate 
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :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                   18.171(3)
_cell_length_b                   18.171
_cell_length_c                   10.987(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      28
_cell_volume                     3627.7(15)
_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 AFC-7S diffractometer'
_diffrn_measurement_method       '2theta-omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2312
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9286
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         .626
_refine_diff_density_min         -.654
_refine_diff_density_rms         .096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2101
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.142
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_obs          0.0511
_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^)+( 0.0828P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1508
_refine_ls_wR_factor_obs         0.1343
_reflns_number_observed          1713
_reflns_number_total             2312
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960158d_4.cif
_cod_data_source_block           lupc2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0828P)^2^+0.0000P] 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^)+( 0.0828P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               4323906