One Step Forward to "Stapled" Bis(phthalocyanine) Metal Complexes: Synthesis, Characterization, and Redox Properties of Bis(phthalocyaninato)niobium(IV). X-ray Crystal Structure of the Monoelectronically Oxidized Species [Pc2Nb](I3)(I2)0.5(ClNP)3.5 (ClNP = 1-Chloronaphthalene)
Maria Pia Donzello; Claudio Ercolani; Angiola Chiesi-Villa; Corrado Rizzoli; Inorganic Chemistry 37 (1998) 1347–1351; doi:10.1021/ic970841f

data_4322702
_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
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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
;
 One Step Forward to "Stapled" Bis(phthalocyanine) Metal Complexes:
 Synthesis, Characterization, and Redox Properties of
 Bis(phthalocyaninato)niobium(IV). X-ray Crystal Structure of the
 Monoelectronically Oxidized Species [Pc2Nb](I3)(I2)0.5(ClNP)3.5 (ClNP =
 1-Chloronaphthalene)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1347
_journal_page_last               1351
_journal_paper_doi               10.1021/ic970841f
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C99 H56.5 Cl3.5 I4 N16 Nb'
_chemical_formula_weight         2194.75
_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           'CIFmaker on Quansan personal computer'
_cell_angle_alpha                106.00(2)
_cell_angle_beta                 93.39(2)
_cell_angle_gamma                83.26(1)
_cell_formula_units_Z            2.00
_cell_length_a                   17.702(3)
_cell_length_b                   18.708(3)
_cell_length_c                   13.504(2)
_cell_measurement_reflns_used    295
_cell_measurement_temperature    25
_cell_measurement_theta_max      16.4
_cell_measurement_theta_min      12.1
_cell_volume                     4267.5(13)
_computing_cell_refinement       'Belletti et al., 1993'
_computing_data_collection       'Belletti, Cantoni & Pasquinell'
_computing_data_reduction        'DIFAU (Belletti et al.)'
_computing_structure_refinement  'SHELXS-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Philips PW1100'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1586
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11865
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.7348
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   'North et al. 1968'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.7080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             2150.0
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.111
_refine_diff_density_min         -.927
_refine_diff_density_rms         .114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.997
_refine_ls_goodness_of_fit_obs   1.129
_refine_ls_hydrogen_treatment    'not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         11764
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_obs          0.0791
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2071
_refine_ls_wR_factor_obs         0.1697
_reflns_number_observed          6490
_reflns_number_total             11865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970841f.cif
_cod_data_source_block           COMPLEX_I
_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^)+(0.0972P)^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^)+(0.0972P)^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_formula_sum        C99H56.5Cl3.5I4N16Nb
_cod_database_code               4322702