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_7119890
_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         'C78 H102 K2 N12 O9'
_chemical_formula_sum            'C78 H102 K2 N12 O9'
_chemical_formula_weight         1429.91
_chemical_name_systematic        5_LE-5-69
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 109.3465(12)
_cell_angle_gamma                90
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_cell_length_b                   12.89091(13)
_cell_length_c                   20.8753(2)
_cell_measurement_reflns_used    15448
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4410
_cell_measurement_theta_min      3.4040
_cell_volume                     4289.56(8)
_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 0.985
_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    -31.00  25.00   1.00    3.00    --   41.04 -57.00  90.00   56
  2  \w     33.00  60.00   1.00    3.00    --   41.04-125.00  60.00   27
  3  \w     33.00  97.00   1.00    3.00    --   41.04-125.00  90.00   64
  4  \w     62.00 106.00   1.00   12.00    --  111.85 -94.00 -60.00   44
  5  \w     93.00 122.00   1.00   12.00    --  111.85-125.00-120.00   29
  6  \w     70.00  95.00   1.00   12.00    --  111.85 -94.00   0.00   25
  7  \w     44.00 131.00   1.00   12.00    --  111.85 -45.00 -90.00   87
  8  \w     85.00 156.00   1.00   12.00    --  111.85  30.00 -90.00   71
  9  \w     97.00 175.00   1.00   12.00    --  111.85  45.00   0.00   78
 10  \w    104.00 178.00   1.00   12.00    --  111.85 125.00-120.00   74
 11  \w    109.00 151.00   1.00   12.00    --  111.85 125.00-150.00   42
 12  \w     92.00 173.00   1.00   12.00    --  111.85  61.00 -60.00   81
 13  \w     99.00 173.00   1.00   12.00    --  111.85 125.00-180.00   74
 14  \w     50.00 125.00   1.00   12.00    --  111.85 -61.00-180.00   75
 15  \w     45.00  81.00   1.00    3.00    --   41.04-125.00-180.00   36
 16  \w     32.00  92.00   1.00   12.00    --  111.85 -94.00-180.00   60
 17  \w     39.00  67.00   1.00   12.00    --  111.85-125.00-120.00   28
 18  \w     89.00 120.00   1.00   12.00    --  111.85-125.00 120.00   31
 19  \w    -67.00  32.00   1.00    3.00    --  -41.04  57.00   0.00   99
 20  \w   -109.00 -27.00   1.00    3.00    --  -41.04 -38.00 120.00   82
 21  \w   -113.00  -9.00   1.00    3.00    --  -41.04 -77.00-120.00  104
;
_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  0.0271
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.053
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.659
_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            yellow
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.158
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.725
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0886
_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^)+(0.1089P)^2^+8.3281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8154
_reflns_number_total             8828
_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        4289.55(8)
_cod_database_code               7119890
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              17900
_shelx_hkl_checksum              51582
_shelx_fab_checksum              3546