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_7119891
_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         'C40 H47 N4 O, Br'
_chemical_formula_sum            'C40 H47 Br N4 O'
_chemical_formula_weight         679.72
_chemical_name_systematic        6_LE-5-55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.0551(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5259(3)
_cell_length_b                   19.9419(3)
_cell_length_c                   29.1694(6)
_cell_measurement_reflns_used    15694
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.6570
_cell_measurement_theta_min      3.7970
_cell_volume                     8292.8(3)
_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      100.01(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 0.982
_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    -65.00  33.00   1.00    4.00    --  -40.91  38.00  60.00   98
  2  \w     20.00 106.00   1.00    4.00    --   40.91  38.00 150.00   86
  3  \w     39.00  83.00   1.00   16.00    --  111.85 -45.00 120.00   44
  4  \w     43.00  83.00   1.00   16.00    --  111.85 -94.00  30.00   40
  5  \w     76.00 121.00   1.00   16.00    --  111.85-125.00 120.00   45
  6  \w     54.00  82.00   1.00    4.00    --   40.91-125.00  60.00   28
  7  \w     30.00 108.00   1.00   16.00    --  111.85 -94.00 -60.00   78
  8  \w     48.00 109.00   1.00   16.00    --  111.85 -94.00-150.00   61
  9  \w     45.00  95.00   1.00    4.00    --   40.91-125.00-120.00   50
 10  \w     42.00 108.00   1.00   16.00    --  111.85-125.00-180.00   66
 11  \w     40.00 138.00   1.00   16.00    --  111.85 -45.00-120.00   98
 12  \w    148.00 178.00   1.00   16.00    --  111.85  15.00 -90.00   30
 13  \w    128.00 167.00   1.00   16.00    --  111.85 103.00   9.00   39
 14  \w    113.00 139.00   1.00   16.00    --  111.85 125.00 -90.00   26
 15  \w    102.00 178.00   1.00   16.00    --  111.85  30.00 -30.00   76
 16  \w     85.00 178.00   1.00   16.00    --  111.85  30.00  60.00   93
 17  \w     64.00 105.00   1.00   16.00    --  111.85  15.00 -90.00   41
 18  \w     45.00 137.00   1.00   16.00    --  111.85 -45.00   0.00   92
 19  \w    -88.00 -21.00   1.00    4.00    --  -40.91 -38.00 150.00   67
 20  \w   -109.00 -16.00   1.00    4.00    --  -40.91 -38.00-120.00   93
;
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            29275
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.948
_diffrn_reflns_theta_min         3.087
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   gaussian
_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            green
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.654
_exptl_crystal_size_mid          0.498
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8514
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+10.9112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8030
_reflns_number_total             8514
_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               7119891
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              48697
_shelx_hkl_checksum              51504
_shelx_fab_checksum              9459