Mixed amido/imido/guanidinato complexes of niobium: potential precursors for MOCVD of niobium nitride thin films
Baunemann, Arne; Bekermann, Daniela; Thiede, Tobias B.; Parala, Harish; Winter, Manuela; Gemel, Christian; Fischer, Roland A.; Dalton Transactions  (2008) 3715–3722; doi:10.1039/b719688a

data_7003792
_publ_section_title
;
 Mixed amido/imido/guanidinato complexes of niobium: potential
 precursors for MOCVD of niobium nitride thin films
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              3715
_journal_page_last               3722
_journal_paper_doi               10.1039/b719688a
_journal_year                    2008
_chemical_formula_sum            'C24 H55 N8 Nb'
_chemical_formula_weight         548.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.094(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.7356(8)
_cell_length_b                   18.2221(4)
_cell_length_c                   18.3713(8)
_cell_measurement_reflns_used    16722
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.53
_cell_volume                     6077.3(4)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '620 images at 1.0 deg. in \w and 30 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61092
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.966
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         13926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0372P)^2^+5.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                10574
_reflns_number_total             13926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719688a.txt
_cod_data_source_block           cvd105
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7003792