Tri-μ-oxido-bis[(5,10,15,20-tetraphenylporphyrinato-κ^4^<i>N</i>)niobium(V)]
Soury, Raoudha; Belkhiria, Mohamed Salah; Daran, Jean-Claude; Nasri, Habib; Acta Crystallographica Section E 67 (2011) m862–m863; doi:10.1107/S1600536811020538

data_2230917
_publ_section_title
;
 Tri-\m-oxido-bis[(5,10,15,20-tetraphenylporphyrinato-\k^4^<i>N</i>)niobium(V)]
;
_journal_coeditor_code           XU5216
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m862
_journal_page_last               m863
_journal_paper_doi               10.1107/S1600536811020538
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Nb2 (C44 H28 N4)2 O3]'
_chemical_formula_moiety         'C88 H56 N8 Nb2 O3'
_chemical_formula_sum            'C88 H56 N8 Nb2 O3'
_chemical_formula_weight         1459.28
_chemical_name_common            niobium(V)-Tri-mu-oxo-tetraphenylporphyrinate
_chemical_name_systematic
;
Tri-\m-oxido-bis[(5,10,15,20-tetraphenylporphyrinato-\k^4^<i>N</i>)niobium(V)]
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 117.823(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.4823(9)
_cell_length_b                   18.4007(8)
_cell_length_c                   14.6257(10)
_cell_measurement_reflns_used    12579
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.1355
_cell_measurement_theta_min      2.9851
_cell_volume                     3446.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'publCIF (Westrip, 2010).'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25553
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            'Dark purple'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.912
_refine_ls_abs_structure_details 'Flack (1983), 2439 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+14.5546P]whereP=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                8244
_reflns_number_total             9945
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5216.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2230917
_cod_database_fobs_code          2230917