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_7027488
_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            'C54.5 H52 Cl N4 O4 Yb'
_chemical_formula_weight         1035.49
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_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           SHELXL-97
_cell_angle_alpha                64.59(1)
_cell_angle_beta                 87.25(1)
_cell_angle_gamma                70.34(1)
_cell_formula_units_Z            2
_cell_length_a                   13.680(1)
_cell_length_b                   14.740(2)
_cell_length_c                   14.969(1)
_cell_measurement_reflns_used    '202 from 4 still frames'
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     2550.9(5)
_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_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
; 

Data was collected to 0.82\%A and 85% completeness by taking 

27 oscillation frames in the range of 0 - 162\%, \D\f = 6\%, 

8 min. per frame.  Crystal to detector distance is 78.150mm, 

background level -100. 

;
_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    0.0618
_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       -18
_diffrn_reflns_number            8136
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  1.122
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0159(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   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          1.203
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+1.2659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                7802
_reflns_number_total             8136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903127hsup1.cif
_cod_data_source_block           5
_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        2550.9(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C54.50 H52 Cl N4 O4 Yb'
_cod_database_code               7027488