The First Nitrosyl Complexes of Niobium and Tantalum
P. James Daff; Peter Legzdins; Steven J. Rettig; Journal of the American Chemical Society 120 (1998) 2688–2689; doi:10.1021/ja9738079

data_4116707
_publ_contact_author_address
;
University of British Columbia
Department of Chemistry
2036 Main Mall
Vancouver, BC V6T 1Z1
Canada
;
_publ_contact_author_email       ' legzdins@chem.ubc.ca '
_publ_contact_author_fax         ' 604-822-2847 '
_publ_contact_author_name        ' Peter Legzdins '
_publ_contact_author_phone       ' 604-822-2471 '
_publ_section_title
;
 The First Nitrosyl Complexes of Niobium and Tantalum
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2688
_journal_page_last               2689
_journal_paper_doi               10.1021/ja9738079
_journal_volume                  120
_journal_year                    1998
_chemical_formula_moiety         'C15 H33 N O3 P3 Si Ta '
_chemical_formula_sum            'C15 H33 N O3 P3 Si Ta'
_chemical_formula_weight         577.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             1997-11-25
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5387(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7532(14)
_cell_length_b                   17.5506(15)
_cell_length_c                   14.2268(5)
_cell_measurement_reflns_used    17441
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     2386.0(4)
_computing_cell_refinement       'd*TREK (MSC, 1997)'
_computing_data_collection       'd*TREK (MSC, 1997)'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      180.2
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03700
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22182
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.863
_exptl_absorpt_correction_T_max  1.004
_exptl_absorpt_correction_T_min  0.358
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.17
_refine_diff_density_min         -2.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.035
_refine_ls_goodness_of_fit_ref   2.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         6039
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0963
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1050
_reflns_number_gt                6039
_reflns_number_total             6039
_reflns_threshold_expression     I>0\s(I)
_cod_data_source_file            ja9738079_2.cif
_cod_data_source_block           compound_4
_cod_original_cell_volume        2386.0(3)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C15 H33 N O3 P3 Si Ta '
_cod_database_code               4116707