Infrared spectroscopic detection of ketene formation from carbene and CO sources: an amide synthesis
Madarasi, Packirisamy Kuzhalmozhi; Sivasankar, Chinnappan; New Journal of Chemistry 44 (2020) 8718–8727; doi:10.1039/C9NJ06161D

data_7059421
_publ_section_title
;
 Infrared spectroscopic detection of ketene formation from carbene and CO
 sources: an amide synthesis
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8718
_journal_page_last               8727
_journal_paper_doi               10.1039/C9NJ06161D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C24 H35 N O3'
_chemical_formula_sum            'C24 H35 N O3'
_chemical_formula_weight         385.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
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_atom_sites_solution_primary     direct
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;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-08-20 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
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'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_measurement_details
;
  1 omega  -80.00  -38.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -      -17.0272  -77.0000   90.0000 42

  2 omega  -31.00    6.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -      -17.0272  -77.0000   60.0000 37

  3 omega  -85.00  -60.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -      -17.0272  -77.0000   60.0000 25

  4 omega  -16.00   34.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -       19.8397  -57.0000 -150.0000 50

  5 omega   -2.00   84.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -       19.8397   57.0000  -30.0000 86

  6 omega  -43.00   -2.00   1.0000   46.0900
omega____ theta____ kappa____ phi______ frames
    -      -17.0272   37.0000   60.0000 41
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
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_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
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_diffrn_source_target            Mo
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_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.074
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_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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    1.1407
_exptl_crystal_description       needle
_exptl_crystal_F_000             840.3857
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_exptl_crystal_size_mid          0.16
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_refine_ls_number_reflns         5325
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_refine_ls_R_factor_all          0.1170
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_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+0.2357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2248
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_reflns_limit_h_min              -13
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_reflns_limit_l_min              0
_reflns_number_gt                3032
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_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9nj06161d2.cif
_cod_data_source_block           CS-PKM-B-132-SS
_cod_depositor_comments
;
 Adding full bibliography for 7059421.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H23.333 N0.667 O2'
_cod_original_formula_weight         257.03
_cod_original_formula_moiety         '0.67(C24 H35 N O3)'
_cod_original_formula_units_Z            6
_cod_database_code               7059421
_chemical_oxdiff_formula         'C18 H20 N O3'
_chemical_oxdiff_usercomment     'COLOURLESS NEEDLE, 298K, 0.8 0.16 0.08'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C12(H12a,H12b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,H16b),
 C18(H18a,H18b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a,H22b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C23(H23), C24(H24), C1a(H1a)
2.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C1b(H1ba,H1bb,H1bc)
;
_olex2_submission_special_instructions 'No special instructions were received'