Structural studies of the whole series of lanthanide double-decker compounds with mixed 2,3-naphthalocyaninato and octaethylporphyrinato ligands
Bian, Yongzhong; Wang, Daqi; Wang, Rongming; Weng, Linhong; Dou, Jianmin; Zhao, Dongyuan; Ng, Dennis K. P.; Jiang, Jianzhuang; New Journal of Chemistry 27 (2003) 844–; doi:10.1039/b209882m

data_7050478
_publ_section_title
;
 Structural studies of the whole series of lanthanide double-decker
 compounds with mixed 2,3-naphthalocyaninato and octaethylporphyrinato
 ligands
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              844
_journal_paper_doi               10.1039/b209882m
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C88 H72 N8 Tm'
_chemical_formula_weight         1410.47
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.632(14)
_cell_length_b                   26.669(13)
_cell_length_c                   10.938(5)
_cell_measurement_reflns_used    1323
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.375
_cell_measurement_theta_min      3.671
_cell_volume                     8352(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35772
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        4.30
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.7324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.419
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00053(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+21.3441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                6416
_reflns_number_total             8392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b209882m.txt
_cod_data_source_block           f11121b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'const' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7050478