Synthesis, structural characterization, and coordination chemistry of imidazole-based alkylidene ketenes.
Feuerstein, Wolfram; Varava, Paul; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Severin, Kay; Chemical communications (Cambridge, England) 57 (2021) 11509–11512; doi:10.1039/d1cc05161j

data_7129128
_publ_section_title
;
 Synthesis, structural characterization, and coordination chemistry of
 imidazole-based alkylidene ketenes.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11509
_journal_page_last               11512
_journal_paper_doi               10.1039/d1cc05161j
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C29 H36 N2 O'
_chemical_formula_sum            'C29 H36 N2 O'
_chemical_formula_weight         428.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8250(4)
_cell_length_b                   8.93762(18)
_cell_length_c                   21.4865(4)
_cell_measurement_reflns_used    3342
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.3620
_cell_measurement_theta_min      5.3920
_cell_volume                     3069.19(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      140.15
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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    -62.00 -37.00   1.00   10.00    --  -40.91 108.00 -99.00   25
  2  \w     28.00  55.00   1.00   10.00    --   40.91-108.00 163.00   27
  3  \w     56.00  84.00   1.00   10.00    --   40.91-108.00 163.00   28
  4  \w    117.00 142.00   1.00   40.00    --  105.15 108.00 -99.00   25
  5  \w    -50.00 -18.00   1.00   10.00    --  -40.91 -38.00-120.00   32
  6  \w   -113.00 -54.00   1.00   10.00    --  -40.91 -38.00-120.00   59
  7  \w    -32.00  65.00   1.00   10.00    --   40.91 -38.00  30.00   97
  8  \w     34.00  81.00   1.00   10.00    --   40.91 -99.00  60.00   47
  9  \w     14.00  39.00   1.00   10.00    --   40.91 -99.00   0.00   25
 10  \w     77.00 126.00   1.00   40.00    --  105.15 -45.00   0.00   49
 11  \w    106.00 157.00   1.00   40.00    --  105.15  77.00-150.00   51
 12  \w    108.00 178.00   1.00   40.00    --  105.15  77.00  60.00   70
 13  \w    105.00 178.00   1.00   40.00    --  105.15 111.00-120.00   73
 14  \w    113.00 177.00   1.00   40.00    --  105.15 111.00  30.00   64
 15  \w     76.00 104.00   1.00   40.00    --  105.15 -94.00-150.00   28
 16  \w    105.00 176.00   1.00   40.00    --  105.15 111.00 150.00   71
 17  \w    113.00 175.00   1.00   40.00    --  105.15 111.00 -30.00   62
 18  \w     79.00 106.00   1.00   40.00    --  105.15 -61.00 -60.00   27
 19  \w     75.00 102.00   1.00   40.00    --  105.15-108.00 163.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3163
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.721
_diffrn_reflns_theta_min         4.332
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3163
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0653P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2346
_reflns_number_total             3163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05161j2.cif
_cod_data_source_block           pv167_final
_cod_depositor_comments
'Adding full bibliography for 7129122--7129133.cif.'
_cod_database_code               7129128
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.699(6)
 0.163(4) 0.138(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: O1(0.5) C3(0.5) C4(0.5)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              6327
_shelx_hkl_checksum              14787
_shelx_fab_checksum              78856
_olex2_submission_special_instructions 'No special instructions were received'