Tetrakis(1,3,4,6,7,8-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-9-ido-κ^2^<i>N</i>^1^,<i>N</i>^9^)niobium(V) hexafluoridophosphate
Cotton, F. Albert; Murillo, Carlos A.; Poplaukhin, Pavel V.; Bhuvanesh, Nattamai; Tiekink, Edward R. T.; Acta Crystallographica Section E 64 (2008) m1197–; doi:10.1107/S1600536808026627

data_2219400
_publ_section_title
;Tetrakis(1,3,4,6,7,8-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-9-ido-\k^2^<i>N</i>^1^,<i>N</i>^9^)niobium(V)
 hexafluoridophosphate
;
_journal_coeditor_code           LX2067
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1197
_journal_paper_doi               10.1107/S1600536808026627
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Nb (C7 H12 N3)4] P F6'
_chemical_formula_moiety         'C28 H48 N12 Nb +, F6 P -'
_chemical_formula_sum            'C28 H48 F6 N12 Nb P'
_chemical_formula_weight         790.66
_chemical_name_systematic
;Tetrakis(1,3,4,6,7,8-hexahydro-2<i>H</i>-pyrimido[1,2-<i>a</i>]pyrimidin-9-ido-
\k^2^<i>N</i>^1^,<i>N</i>^9^)niobium(V)
 hexafluoridophosphate
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.531(6)
_cell_length_b                   13.531(6)
_cell_length_c                   9.159(4)
_cell_measurement_reflns_used    10356
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     1676.9(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10356
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0498
_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^)+(0.067P)^2^+3.4248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                1381
_reflns_number_total             1655
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2067.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               2219400
_cod_database_fobs_code          2219400