The Intra- and Intermolecular Oxidative Coupling of Ni(II)-meso-Octaethyl Mono(pyridine)-Tris(pyrrole) Complex Leading to CC Bonds: Pathways to Oligomeric Porphyrinogens
Raffaella Crescenzi; Euro Solari; Carlo Floriani; Angiola Chiesi-Villa; Corrado Rizzoli; Inorganic Chemistry 37 (1998) 6044–6051; doi:10.1021/ic9806378

data_4323169
_publ_contact_author
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     Dr. Corrado Rizzoli
     Universit\'a di Parma
     Dipartimento di Chimica Generale ed Inorganica,
     Chimica Analitica, Chimica Fisica
     Viale delle Scienze 78
     I-43100 Parma
     Italy
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_publ_contact_author_email       rizzoli@at@ipruniv.cce.unipr.it
_publ_contact_author_fax         '[039]521 905 556'
_publ_contact_author_phone       '[039]521 905 449'
_publ_section_title
;
 The Intra- and Intermolecular Oxidative Coupling of Ni(II)-meso-Octaethyl
 Mono(pyridine)-Tris(pyrrole) Complex Leading to CC Bonds: Pathways to
 Oligomeric Porphyrinogens
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6044
_journal_page_last               6051
_journal_paper_doi               10.1021/ic9806378
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C78 H108 N8 Ni2 O'
_chemical_formula_weight         1291.18
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 106.02(3)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   15.999(3)
_cell_length_b                   16.855(3)
_cell_length_c                   27.157(5)
_cell_measurement_reflns_used    295
_cell_measurement_temperature    200
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      8.2
_cell_volume                     7039(2)
_computing_cell_refinement       'STOE Program Package'
_computing_data_collection       'STOE Program Package'
_computing_data_reduction        'STOE Program Package'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0582
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_exptl_absorpt_coefficient_mu    0.5845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.2184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
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_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.046
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_refine_ls_hydrogen_treatment    not_refined
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0989
_refine_ls_wR_factor_obs         0.0875
_reflns_number_observed          4278
_reflns_number_total             5554
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9806378_5.cif
_cod_data_source_block           COMPLEX9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0621P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7039.(2)
_cod_original_formula_sum        C78H108N8Ni2O
_cod_database_code               4323169