Synthesis, characterization and crystal structures of neutral mono- and di-nuclear lanthanide(III) porphyrinate complexes
Wong, Wai-Kwok; Zhang, Lilu; Xue, Feng; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (1999) 3053–; doi:10.1039/a903127h

data_7027485
_publ_section_title
;
 Synthesis, characterization and crystal structures of neutral mono- and
 di-nuclear lanthanide(III) porphyrinate complexes
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3053
_journal_paper_doi               10.1039/a903127h
_journal_year                    1999
_chemical_formula_sum            'C100 H87 Cl2 N8 O6.5 Y2'
_chemical_formula_weight         1753.50
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           Manual
_cell_angle_alpha                63.95(2)
_cell_angle_beta                 87.14(2)
_cell_angle_gamma                71.12(2)
_cell_formula_units_Z            1
_cell_length_a                   13.607(2)
_cell_length_b                   14.732(2)
_cell_length_c                   14.933(2)
_cell_measurement_reflns_used    '91 from 4 still frames'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2529.6(9)
_computing_cell_refinement       'BioteX 1.0 (MSC, 1990)'
_computing_data_collection       'BioteX 1.0 (MSC, 1990)'
_computing_data_reduction        'BioteX 1.0 (MSC, 1990)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;

Data was collected to 0.82\%A and 80% completeness by taking

36 oscillation frames in the range of 0 - 180\%, \D\f = 5\%,

10 min. per frame.  Crystal to detector distance is 77.766 mm,

background level -30.

;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;

Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA

;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1100
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6225
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  1.149
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             907
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.35
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.33
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         3532
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo) + 0.0050Fo^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1863
_reflns_number_gt                3532
_reflns_number_total             6255
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            903127hsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2529.6(3)
_cod_original_sg_symbol_H-M      P1
_cod_original_formula_sum        'C100 H87 Cl2 N8 O6.50 Y2'
_cod_database_code               7027485