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_7003793
_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            'C30 H67 N8 Nb'
_chemical_formula_weight         632.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4815(9)
_cell_length_b                   18.2528(18)
_cell_length_c                   34.814(3)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.58
_cell_volume                     7296.0(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '560 images at 1.0 deg. in \w and 35 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  0.1846
_diffrn_reflns_av_sigmaI/netI    0.1508
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            56871
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.0964
_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^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                4000
_reflns_number_total             6417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719688a.txt
_cod_data_source_block           cvd81
_cod_original_cell_volume        7295.9(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7003793