Adducts of Nitrous Oxide and N-Heterocyclic Carbenes: Syntheses, Structures, and Reactivity
Alexander G. Tskhovrebov; Basile Vuichoud; Euro Solari; Rosario Scopelliti; Kay Severin; Journal of the American Chemical Society 135 (2013) 9486–9492; doi:10.1021/ja4030287

data_4119985
_publ_section_title
;
 Adducts of Nitrous Oxide and N-Heterocyclic Carbenes: Syntheses,
 Structures, and Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9486
_journal_page_last               9492
_journal_paper_doi               10.1021/ja4030287
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C51 H64 F3 Fe N8 O7 S, C F3 O3 S, 3/2(C4 H8 O)'
_chemical_formula_sum            'C58 H76 F6 Fe N8 O11.5 S2'
_chemical_formula_weight         1303.24
_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
_audit_update_record
;
2013-03-14 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.440(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2126(10)
_cell_length_b                   16.522(3)
_cell_length_c                   34.824(5)
_cell_measurement_reflns_used    445
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     6422.2(16)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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      160(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            83831
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         11952
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0435P)^2^+8.4220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                10252
_reflns_number_total             11952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4030287_si_013.cif
_cod_data_source_block           al394
_cod_original_cell_volume        6422.2(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C58 H76 F6 Fe N8 O11.50 S2'
_cod_database_code               4119985