"Stapled" Bis(phthalocyaninato)niobium(IV), Pc2Nb: X-ray Crystal Structure, Chemical and Electrochemical Behavior, and Theoretical Studies. Perspectives for the Use of Pc2Nb (Thin Films) as an "Optically Passive Electrode" in Electrochromic Devices
Elvira M. Bauer; Maria Pia Donzello; Claudio Ercolani; Enrico Masetti; Stefania Panero; Giampaolo Ricciardi; Angela Rosa; Angiola Chiesi-Villa; Corrado Rizzoli; Inorganic Chemistry 42 (2003) 283–293; doi:10.1021/ic020098d

data_4312911
_publ_contact_author
;
      Prof. Corrado Rizzoli
      Universita di Parma
      Dipartimento di Chimica Generale ed Inorganica
      Chimica Analitica, Chimica Fisica
      Viale delle Scienze 17/A
      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
;
 "Stapled" Bis(phthalocyaninato)niobium(IV), Pc2Nb: X-ray Crystal
 Structure, Chemical and Electrochemical Behavior, and Theoretical
 Studies. Perspectives for the Use of Pc2Nb (Thin Films) as an "Optically
 Passive Electrode" in Electrochromic Devices
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              283
_journal_page_last               293
_journal_paper_doi               10.1021/ic020098d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C99 H56.5 Cl3.5 N16 Nb'
_chemical_formula_weight         1687.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             05/02/2002
_audit_creation_method           'ModiCIF v1.02'
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 92.51(2)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   16.765(3)
_cell_length_b                   23.800(4)
_cell_length_c                   19.421(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      14.6
_cell_volume                     7742(2)
_computing_cell_refinement       'Belletti et al., 1993'
_computing_data_collection       'Belletti, Cantoni & Pasquinelli,1993'
_computing_data_reduction        'DIFAU (Belletti et al.)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.1305
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21100
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.3405
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.4475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             3452.0
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.884
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    not_refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         16772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_obs          0.0524
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1411
_refine_ls_wR_factor_obs         0.1222
_reflns_number_observed          9037
_reflns_number_total             20074
_reflns_threshold_expression     '>2 sigma(I)'
_cod_data_source_file            ic020098d.cif
_cod_data_source_block           Complex1
_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^)+(0.0693P)^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^)+(0.0693P)^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        'C99 H56.5Cl3.5 N16Nb1'
_cod_database_code               4312911