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_7119889
_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         'C34 H42 N4 O, C H4 O'
_chemical_formula_sum            'C35 H46 N4 O2'
_chemical_formula_weight         554.76
_chemical_name_systematic        4_le-5-7
_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                 101.3468(19)
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_cell_length_c                   20.6981(4)
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_cell_measurement_temperature    140.00(10)
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_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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     13.00  58.00   1.00    1.46    --   40.91  57.00 -60.00   45
  2  \w     92.00 118.00   1.00    5.83    --  111.85 -45.00 -60.00   26
  3  \w     72.00 144.00   1.00    5.83    --  111.85 -77.00-180.00   72
  4  \w     40.00 137.00   1.00    5.83    --  111.85 -61.00   0.00   97
  5  \w     72.00 126.00   1.00    5.83    --  111.85 -45.00 120.00   54
  6  \w     86.00 169.00   1.00    5.83    --  111.85  45.00  90.00   83
  7  \w     87.00 154.00   1.00    5.83    --  111.85  61.00 150.00   67
  8  \w     41.00  88.00   1.00    5.83    --  111.85 -45.00 -60.00   47
  9  \w     25.00  79.00   1.00    1.46    --   40.91-125.00-150.00   54
 10  \w    -69.00 -11.00   1.00    1.46    --  -40.91  57.00  90.00   58
 11  \w   -117.00 -33.00   1.00    1.46    --  -40.91 -77.00 -30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
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_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.920
_diffrn_reflns_theta_min         4.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.893
_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            purple
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.273
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6556
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.9652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5329
_reflns_number_total             6556
_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_original_cell_volume        3239.32(10)
_cod_database_code               7119889
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              85934
_shelx_hkl_checksum              1327