Niobium-nitrides derived from nitrogen splitting
Keith Searles; Patrick J. Carroll; Chun-Hsing Chen; Maren Pink; Daniel J. Mindiola; Chem.Commun. 51 (2015) 3526–; doi:10.1039/C4cc09563D

data_7116548
_publ_section_title
;
 Niobium-nitrides derived from nitrogen splitting
;
_journal_name_full               Chem.Commun.
_journal_page_first              3526
_journal_paper_doi               10.1039/C4cc09563D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C151 H140 N2 Nb2 O4'
_chemical_formula_weight         2232.47
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-04 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.6450(6)
_cell_length_b                   25.8062(5)
_cell_length_c                   37.2338(8)
_cell_measurement_temperature    100(1)
_cell_volume                     23680.5(9)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3233
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            407228
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9392
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.504
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         27382
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.2176
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+146.2397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2415
_refine_ls_wR_factor_ref         0.3249
_reflns_number_gt                12036
_reflns_number_total             27382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09563d2.cif
_cod_data_source_block           shelxl_b
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               7116548