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_4323903
_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 N17 Nd'
_chemical_formula_weight         1411.75
_chemical_name_systematic
; 
tetrabutylammonium bis(phtahlocyaninato)-neodymium(iii) 
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :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            4
_cell_length_a                   17.0545(6)
_cell_length_b                   17.0545(6)
_cell_length_c                   22.807(3)
_cell_measurement_temperature    296(2)
_cell_volume                     6633.6(9)
_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  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16457
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.15
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_type   n
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       prism
_exptl_crystal_F_000             2908
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .518
_refine_diff_density_min         -.764
_refine_diff_density_rms         .076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.147
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3239
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.170
_refine_ls_restrained_S_obs      1.151
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_obs          0.0506
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0649P)^2^+9.0573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1663
_refine_ls_wR_factor_obs         0.1297
_reflns_number_observed          2428
_reflns_number_total             3741
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960158d_1.cif
_cod_data_source_block           ndpc2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0649P)^2^+9.0573P] 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^)+( 0.0649P)^2^+9.0573P] 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        6633.6(10)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4323903