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_4323905
_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 Ho N17 O'
_chemical_formula_weight         1450.46
_chemical_name_systematic
; 
tetrabutylammonium bis(phtahlocyaninato)-holmium(iii) water solvate  
;
_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                   18.096(5)
_cell_length_b                   18.096
_cell_length_c                   11.079(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     3628(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SAPI-91 (Fan Hai-Fu, 1988)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Rigaku AFC-5R diffractmeter'
_diffrn_measurement_method       '2theta-omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0580
_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            2420
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9585
_exptl_absorpt_correction_type   \y-scan
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.480
_refine_diff_density_min         -.535
_refine_diff_density_rms         .150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.262
_refine_ls_restrained_S_obs      1.189
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         -0.171
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0991P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1969
_refine_ls_wR_factor_obs         0.1474
_reflns_number_observed          1594
_reflns_number_total             2420
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960158d_3.cif
_cod_data_source_block           hopc2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0991P)^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^)+( 0.0991P)^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_cell_volume        3628.0(22)
_cod_database_code               4323905