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_7116549
_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_moiety         'C144 H132 Cl6 Nb2 O4, 3(C7 H8)'
_chemical_formula_sum            'C165 H156 Cl6 Nb2 O4'
_chemical_formula_weight         2601.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                 93.396(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.1297(8)
_cell_length_b                   15.6334(8)
_cell_length_c                   26.0900(12)
_cell_measurement_reflns_used    3483
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.92
_cell_measurement_theta_min      4.88
_cell_volume                     7381.7(6)
_computing_cell_refinement       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_collection       'APEX II v2010.11.3 (Bruker, 2013)'
_computing_data_reduction        'APEX II v2010.11.3 (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2010)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
'0.50 degree frames measured for 60 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44783
_diffrn_reflns_theta_full        61.31
_diffrn_reflns_theta_max         61.31
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.110
_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     811
_refine_ls_number_reflns         11303
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1235P)^2^+8.2346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2116
_reflns_number_gt                8070
_reflns_number_total             11303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09563d2.cif
_cod_data_source_block           12039
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7116549