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_7027487
_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 H82.5 N8 O3.25 Yb2'
_chemical_formula_weight         1794.32
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 108.09(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.758(1)
_cell_length_b                   27.758(1)
_cell_length_c                   20.303(1)
_cell_measurement_reflns_used    '132 from 4 still photos'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2
_cell_measurement_theta_min      26
_cell_volume                     8977.5(9)
_computing_cell_refinement       'BioteX 1.0 (MSC, 1995)'
_computing_data_collection       'BioteX 1.0 (MSC, 1995)'
_computing_data_reduction        'BioteX 1.0 (MSC, 1995)'
_computing_molecular_graphics    '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 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;

Data was collected at 0.82\%A and 88% completeness by taking

60 oscillation frames in the range of 0 - 180\%, \D\f = 3\%,

8 min. per frame.  Crystal to detector distance is 77.865mm,

background level -80.

;
_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    0.0786
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12384
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_T_max  1.194
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3618
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00000(3)
_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   1.235
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         12384
_refine_ls_number_restraints     1159
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.145
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+79.9221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1872
_reflns_number_gt                11177
_reflns_number_total             12384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903127hsup1.cif
_cod_data_source_block           4
_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 'Monoclinic' changed to 'monoclinic'
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        8977.5(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C100 H82.50 N8 O3.25 Yb2'
_cod_database_code               7027487