Solid-State 17O NMR and Computational Studies of C-Nitrosoarene Compounds
Gang Wu; Jianfeng Zhu; Xin Mo; Ruiyao Wang; Victor Terskikh; Journal of the American Chemical Society 132 (2010) 5143–5155; doi:10.1021/ja909656w

data_4102264
_publ_section_title
;
 Solid-State 17O NMR and Computational Studies of C-Nitrosoarene Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5143
_journal_page_last               5155
_journal_paper_doi               10.1021/ja909656w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C18 H26 Cl2 N4 O2 Sn'
_chemical_formula_weight         520.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.5200(10)
_cell_angle_beta                 109.2810(10)
_cell_angle_gamma                91.8730(10)
_cell_formula_units_Z            1
_cell_length_a                   7.11490(10)
_cell_length_b                   8.7177(2)
_cell_length_c                   9.2105(2)
_cell_measurement_reflns_used    4124
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.28
_cell_measurement_theta_min      3.04
_cell_volume                     538.836(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4018
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.7944
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         1839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0151
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.1387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                1822
_reflns_number_total             1839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909656w_si_002.cif
_cod_data_source_block           wu02
_cod_database_code               4102264