White Phosphorus Activation at a Metal-Phosphorus Triple Bond: a New Route to cyclo-Triphosphorus or cyclo-Pentaphosphorus Complexes of Niobium
Daniel Tofan; Brandi M. Cossairt; Christopher C. Cummins; Inorganic Chemistry 50 (2011) 12349–12358; doi:10.1021/ic2014607

data_4327087
_publ_section_title
;
 White Phosphorus Activation at a Metal-Phosphorus Triple Bond: a New
 Route to cyclo-Triphosphorus or cyclo-Pentaphosphorus Complexes of
 Niobium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12349
_journal_page_last               12358
_journal_paper_doi               10.1021/ic2014607
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C63 H108 N3 Na Nb O6 P5'
_chemical_formula_weight         1274.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 107.7930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.936(4)
_cell_length_b                   12.7624(10)
_cell_length_c                   25.324(2)
_cell_measurement_reflns_used    9383
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.27
_cell_volume                     14136(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            118612
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.9358
_exptl_absorpt_correction_T_min  0.8237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       shard
_exptl_crystal_F_000             5456
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         28903
_refine_ls_number_restraints     5058
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+19.1580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                23588
_reflns_number_total             28903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2014607_si_001.cif
_cod_data_source_block           09117-NbP5
_cod_original_cell_volume        14136.0(19)
_cod_database_code               4327087