Synthesis, structure and near-infrared luminescence of neutral 3dâ€“4f bi-metallic monoporphyrinate complexes
Wong, Wai-Kwok; Hou, Anxin; Guo, Jianping; He, Hongshan; Zhang, Lilu; Wong, Wai-Yeung; Li, King-Fai; Cheah, Kok-Wai; Xue, F.; Mak, Thomas C. W.; Journal of the Chemical Society, Dalton Transactions  (2001) 3092–; doi:10.1039/b104993n

data_7010889
_publ_section_title
;
 Synthesis, structure and near-infrared luminescence of neutral
 3d\^a&#x20AC;&#x201C;4f bi-metallic monoporphyrinate complexes
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3092
_journal_paper_doi               10.1039/b104993n
_journal_year                    2001
_chemical_formula_sum            'C67.25 H75.5 Co N4 O13.75 P3 Yb'
_chemical_formula_weight         1484.70
_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                79.35(3)
_cell_angle_beta                 86.77(3)
_cell_angle_gamma                74.81(3)
_cell_formula_units_Z            2
_cell_length_a                   12.827(3)
_cell_length_b                   14.337(3)
_cell_length_c                   22.294(5)
_cell_measurement_reflns_used    151
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3888.4(16)
_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 (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.851
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Data was collected to 0.82\%A and 85% completeness by taking
47 oscillation frames in the range of 0 - 180\%, \D\f = 5\%
or 2.5\%, 8 min. per frame.  Crystal to detector distance is
78.069 mm, 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    0.0686
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12368
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  1.106
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0110(6)
_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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         12368
_refine_ls_number_restraints     676
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0567
_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^)+(0.1112P)^2^+0.4915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                11575
_reflns_number_total             12368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104993n.txt
_cod_data_source_block           XF153
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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        3888.4(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C67.25 H75.50 Co N4 O13.75 P3 Yb'
_cod_database_code               7010889