Unpicking the determinants of amide NH••O=C hydrogen bond strength with diphenylacetylene molecular balances
Luccarelli, James; Jones, Ian M.; Thompson, Sam; Hamilton, Andrew D.; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB02026K

data_7155900
_publ_section_title
;
 Unpicking the determinants of amide NH&#x2022;&#x2022;O=C hydrogen bond
 strength with diphenylacetylene molecular balances
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB02026K
_journal_year                    2017
_chemical_formula_moiety         'C24.50 H20.50 Cl1.50 N2 O4 '
_chemical_formula_sum            'C24.5 H20.5 Cl1.5 N2 O4'
_chemical_formula_weight         460.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_update_record
;
2017-07-31 deposited with the CCDC.
2017-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                59.3789(7)
_cell_angle_beta                 76.9217(8)
_cell_angle_gamma                68.9074(9)
_cell_formula_units_Z            2
_cell_length_a                   8.47250(15)
_cell_length_b                   12.5302(2)
_cell_length_c                   12.5601(2)
_cell_measurement_reflns_used    13292
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      65.1
_cell_measurement_theta_min      6.8
_cell_volume                     1069.05(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      93.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14013
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_T_min  0.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             478.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.24
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     320
_refine_ls_number_reflns         3408
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0821P)^2^+2.0445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                3123
_reflns_number_total             3408
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7ob02026k2.cif
_cod_data_source_block           '_ij04'
_cod_original_cell_volume        1069.06(3)
_cod_original_formula_sum        'C24.50 H20.50 Cl1.50 N2 O4 '
_cod_database_code               7155900