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_4323165
_publ_contact_author
;
     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
;
_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
;
_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            'C41 H57 Li N4 O'
_chemical_formula_weight         628.87
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                99.07(2)
_cell_angle_beta                 113.88(3)
_cell_angle_gamma                71.87(2)
_cell_formula_units_Z            2.00
_cell_length_a                   11.815(2)
_cell_length_b                   15.94(3)
_cell_length_c                   11.26(2)
_cell_measurement_reflns_used    143
_cell_measurement_temperature    25
_cell_measurement_theta_max      64.0
_cell_measurement_theta_min      43.3
_cell_volume                     1842(5)
_computing_cell_refinement       'TEXSAN Software'
_computing_data_collection       'TEXSAN Software'
_computing_data_reduction        'TEXSAN Software'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7253
_diffrn_reflns_theta_max         70.15
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.4832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   'North et al. 1968'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.1339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       elongated_prism
_exptl_crystal_F_000             684.0
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.074
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_hydrogen_treatment    not_refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.214
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_obs          0.0636
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1112P)^2^+0.0152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2309
_refine_ls_wR_factor_obs         0.1705
_reflns_number_observed          3512
_reflns_number_total             6890
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9806378_1.cif
_cod_data_source_block           COMPLEX11
_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^)+(
0.1112P)^2^+0.0152P] 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^)+( 0.1112P)^2^+0.0152P] 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        1842.(5)
_cod_original_formula_sum        C41H57LiN4O
_cod_database_code               4323165