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_7116547
_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            'C149 H144 Cl5 K3 Nb2 O4'
_chemical_formula_weight         2479.01
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                92.288(4)
_cell_angle_beta                 100.453(4)
_cell_angle_gamma                114.629(4)
_cell_formula_units_Z            2
_cell_length_a                   16.7009(14)
_cell_length_b                   17.9962(15)
_cell_length_c                   24.535(2)
_cell_measurement_temperature    100(1)
_cell_volume                     6536.7(10)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            161655
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.538
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1483
_refine_ls_number_reflns         30335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+9.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                24323
_reflns_number_total             30335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09563d2.cif
_cod_data_source_block           shelxl_a
_cod_original_cell_volume        6536.7(9)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               7116547