Porphyrinogen tetraanion functioning as a polymetallic assembler: nickel-meso-octaethylporphyrinogen binding four transition metal ions at the periphery
Bonomo, Lucia; Solari, Euro; Martin, Géraldine; Scopelliti, Rosario; Floriani, Carlo; Chemical Communications  (1999) 2319–; doi:10.1039/a907268c

data_7110710
_publ_section_title
;
 Porphyrinogen tetraanion functioning as a polymetallic assembler:
 nickel-meso-octaethylporphyrinogen binding four transition metal ions at
 the periphery
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2319
_journal_paper_doi               10.1039/a907268c
_journal_year                    1999
_chemical_formula_moiety         'C62 H88 Li2 Mo2 N4 Ni O11, C4 H8 O'
_chemical_formula_sum            'C66 H96 Li2 Mo2 N4 Ni O12'
_chemical_formula_weight         1401.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.537(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   50.392(4)
_cell_length_b                   11.6140(8)
_cell_length_c                   23.8148(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      5
_cell_volume                     13428.4(16)
_computing_cell_refinement
'CrysAlis RED, Kuma Diffraction Instruments GmbH, release 1.6.0, 1999'
_computing_data_collection
'CrysAlis CCD, Kuma Diffraction Instruments GmbH, release 1.6.0, 1999'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
'SHELXTL, Bruker AXS, Inc., release 5.1, 1997'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97 (Altomare A. et al., J. Appl. Cryst., 1999, 32, 115-119)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device_type
'KUMA diffractometer equipped with a CCD detector'
_diffrn_measurement_method
'2 runs (110 frames each) using omega scan, 1 run (300 frames) using phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38408
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5872
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.00016(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   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11199
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+131.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                9809
_reflns_number_total             11199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907268csup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
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        13428.3(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7110710