Fixation of nitrous oxide by mesoionic and carbanionic N-heterocyclic carbenes.
Eymann, Léonard Y M; Scopelliti, Rosario; Fadaei, Farzaneh T.; Cecot, Giacomo; Solari, Euro; Severin, Kay; Chemical communications (Cambridge, England) 53 (2017) 4331–4334; doi:10.1039/c7cc01592e

data_7119888
_publ_section_title
;
 Fixation of nitrous oxide by mesoionic and carbanionic N-heterocyclic
 carbenes.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4331
_journal_page_last               4334
_journal_paper_doi               10.1039/c7cc01592e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C33 H40 N4 O, 2(C H4 O)'
_chemical_formula_sum            'C35 H48 N4 O3'
_chemical_formula_weight         572.77
_chemical_name_systematic        3a_le-5-2
_chemical_properties_physical    ', Heat-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-15 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0138(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0226(3)
_cell_length_b                   11.73248(17)
_cell_length_c                   19.0842(3)
_cell_measurement_reflns_used    10334
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.8610
_cell_measurement_theta_min      4.3140
_cell_volume                     3248.81(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -58.00  26.00   1.00    4.05    --  -40.91  38.00   0.00   84
  2  \w    -64.00  22.00   1.00    4.05    --  -40.91  57.00-180.00   86
  3  \w     32.00  86.00   1.00    4.05    --   40.91-125.00 -90.00   54
  4  \w     55.00 101.00   1.00   16.22    --  111.85 -94.00 -60.00   46
  5  \w     83.00 115.00   1.00   16.22    --  111.85-125.00 -90.00   32
  6  \w     78.00 138.00   1.00   16.22    --  111.85 -45.00-120.00   60
  7  \w     91.00 171.00   1.00   16.22    --  111.85  30.00-180.00   80
  8  \w    150.00 176.00   1.00   16.22    --  111.85  61.00-180.00   26
  9  \w    112.00 138.00   1.00   16.22    --  111.85  61.00-180.00   26
 10  \w     98.00 176.00   1.00   16.22    --  111.85  45.00 -90.00   78
 11  \w     88.00 133.00   1.00   16.22    --  111.85  45.00 -30.00   45
 12  \w     82.00 166.00   1.00   16.22    --  111.85  77.00-150.00   84
 13  \w     43.00  70.00   1.00   16.22    --  111.85 -45.00-120.00   27
 14  \w     41.00 134.00   1.00   16.22    --  111.85 -61.00  30.00   93
 15  \w     75.00 105.00   1.00   16.22    --  111.85 -94.00 120.00   30
 16  \w     57.00 122.00   1.00   16.22    --  111.85-125.00  60.00   65
 17  \w     40.00 128.00   1.00   16.22    --  111.85 -61.00 150.00   88
 18  \w     41.00  67.00   1.00   16.22    --  111.85-125.00 150.00   26
 19  \w     30.00  94.00   1.00    4.05    --   40.91-125.00  90.00   64
 20  \w   -129.00 -17.00   1.00    4.05    --  -40.91   0.00   0.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.152
_diffrn_reflns_theta_min         4.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+1.9191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5825
_reflns_number_total             6696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01592e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7119887--7119892.cif.'
_cod_database_code               7119888
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              90495
_shelx_hkl_checksum              44151