Substituent Effects in CH Hydrogen Bond Interactions: Linear Free Energy Relationships and Influence of Anions.
Tresca, Blakely W.; Hansen, Ryan J.; Chau, Calvin V.; Hay, Benjamin P.; Zakharov, Lev N.; Haley, Michael M.; Johnson, Darren W.; Journal of the American Chemical Society 137 (2015) 14959–14967; doi:10.1021/jacs.5b08767

data_4129607
_publ_section_title
;
 Substituent Effects in CH Hydrogen Bond Interactions: Linear Free Energy
 Relationships and Influence of Anions.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14959
_journal_page_last               14967
_journal_paper_doi               10.1021/jacs.5b08767
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C47 H46.5 N5.5 O6'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yc'
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_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
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_cell_angle_beta                 101.756(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7165(16)
_cell_length_b                   9.0824(8)
_cell_length_c                   29.495(3)
_cell_measurement_reflns_used    3464
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      49.44
_cell_measurement_theta_min      3.06
_cell_volume                     4384.2(7)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.551
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.551
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
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_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15027
_diffrn_reflns_point_group_measured_fraction_full 0.551
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.199
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.6034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       needle
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         4362
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.1023
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1491P)^2^+15.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2840
_refine_ls_wR_factor_ref         0.3018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3181
_reflns_number_total             4362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08767_si_002.cif
_cod_data_source_block           cu_dwjr180_0m
_cod_original_cell_volume        4384.2(8)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'C47 H46.50 N5.50 O6'
_cod_database_code               4129607
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.981
_shelxl_version_number           2013-4
_shelx_res_checksum              16230
_shelx_hkl_checksum              72080