Creating skeletal complexity through an interrupted Corey-Chaykovsky reaction of activated alkynes.
Yadav, Nisha; Ramasastry, S. S. V.; Chemical communications (Cambridge, England) 61 (2025) 15179–15182; doi:10.1039/d5cc04277a

data_7134930
_publ_section_title
;
 Creating skeletal complexity through an interrupted Corey-Chaykovsky
 reaction of activated alkynes.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15179
_journal_page_last               15182
_journal_paper_doi               10.1039/d5cc04277a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C26 H19 N O'
_chemical_formula_sum            'C26 H19 N O'
_chemical_formula_weight         361.447
_chemical_name_systematic        'ny 01 343'
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-18 deposited with the CCDC.	2025-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.895(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2995(7)
_cell_length_b                   14.7508(9)
_cell_length_c                   13.5318(10)
_cell_measurement_reflns_used    4325
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.0090
_cell_measurement_theta_min      3.1390
_cell_volume                     1967.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9483
_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    -69.00 118.20   0.30    7.56    --   29.89  54.00  30.00  624
  2  \w    -69.00 118.20   0.30    7.56    --   29.89  54.00 150.00  624
  3  \w    -69.00  12.00   0.30    7.56    --   29.89  54.00 -90.00  270
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0384815000
_diffrn_orient_matrix_UB_12      -0.0199644000
_diffrn_orient_matrix_UB_13      -0.0471817000
_diffrn_orient_matrix_UB_21      0.0399201000
_diffrn_orient_matrix_UB_22      -0.0398793000
_diffrn_orient_matrix_UB_23      0.0122322000
_diffrn_orient_matrix_UB_31      -0.0459140000
_diffrn_orient_matrix_UB_32      -0.0179504000
_diffrn_orient_matrix_UB_33      0.0250674000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9483
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22403
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9483
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.82
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             760.431
_exptl_crystal_preparation       'done in isopropanol:hexane'
_exptl_crystal_recrystallization_method 'done at rt in isopropanol:hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4618
_refine_diff_density_min         -0.3438
_refine_diff_density_rms         0.0786
_refine_ls_d_res_high            0.6556
_refine_ls_d_res_low             7.8321
_refine_ls_goodness_of_fit_ref   1.2212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     254
_refine_ls_number_reflns         6951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.2212
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.2110
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4371
_reflns_number_total             6951
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc04277a2.cif
_cod_data_source_block           NY-01-343
_cod_depositor_comments          'Adding full bibliography for 7134930.cif.'
_cod_original_cell_volume        1967.1(3)
_cod_database_code               7134930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C004(H004), C00D(H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S)
2.c Idealised Me refined as rotating group:
 C00O(H00a,H00b,H00c)
;
_olex2_submission_original_sample_id 'ny 01 343'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.785
_oxdiff_exptl_absorpt_empirical_full_min 0.747