Nitrosonium Complexes of Resorc[4]arenes: Spectral, Kinetic, and Theoretical Studies
Bruno Botta; Ilaria D'Acquarica; Giuliano Delle Monache; Laura Nevola; Danila Tullo; Franco Ugozzoli; Marco Pierini; Journal of the American Chemical Society 129 (2007) 11202–11212; doi:10.1021/ja072855i

data_4109894
_publ_section_title
;
 Nitrosonium Complexes of Resorc[4]arenes: Spectral, Kinetic, and
 Theoretical Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11202
_journal_page_last               11212
_journal_paper_doi               10.1021/ja072855i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C56 H72 O18'
_chemical_formula_weight         1033.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                101.070(8)
_cell_angle_beta                 88.617(6)
_cell_angle_gamma                108.563(9)
_cell_formula_units_Z            1
_cell_length_a                   12.264(9)
_cell_length_b                   14.080(2)
_cell_length_c                   8.4440(10)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41
_cell_measurement_theta_min      20
_cell_volume                     1355.4(10)
_computing_cell_refinement       'DIPCHIGE software package 2004'
_computing_data_collection       'DIPCHIGE software package 2004'
_computing_data_reduction        DIFAU92
_computing_molecular_graphics    'Accelrys DS-ViewerPro 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 1Kev
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens AED'
_diffrn_measurement_method       'scintil counter'
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5500
_diffrn_reflns_theta_full        70.21
_diffrn_reflns_theta_max         70.21
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.11
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       'thick column'
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         5366
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.1976
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2526
_reflns_number_gt                1935
_reflns_number_total             5366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072855irom20070502_093454.cif
_cod_data_source_block           bot207
_cod_database_code               4109894