Synthesis and X-ray crystal structure of an unexpected neutral oxalate-bridged ytterbium(III) porphyrinate dimer
Wong, Wai-Kwok; Zhang, Li-Lu; Xue, Feng; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (2000) 2245–; doi:10.1039/b003434g

data_7009756
_publ_section_title
;
 Synthesis and X-ray crystal structure of an unexpected neutral
 oxalate-bridged ytterbium(III) porphyrinate dimer
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2245
_journal_paper_doi               10.1039/b003434g
_journal_year                    2000
_chemical_formula_sum            'C55 H53 N4 O7 Yb'
_chemical_formula_weight         1055.05
_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                 103.2(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.646(1)
_cell_length_b                   23.715(3)
_cell_length_c                   17.944(2)
_cell_measurement_reflns_used    '221 from 4 still frames'
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     5239(2)
_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    'XP in SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
; 
Data was collected to 0.82\%A with 88% completeness by taking 
41 oscillation photos in the range of 0 - 164\%, \D\f = 4\%, 
8 min. per frame.  Crystal to detector distance is 78.098 mm, 
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  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14941
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  1.092
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.321
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0034(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   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8594
_refine_ls_number_restraints     335
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                7715
_reflns_number_total             8594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003434g.txt
_cod_data_source_block           xf142
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5239.2(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009756