Direct Observation of the Symmetrical and Asymmetrical Protonation States in Molecular Crystals.
Ma, Suqian; Zhang, Jibo; Liu, Yingjie; Qian, Jingyu; Xu, Bin; Tian, Wenjing; The journal of physical chemistry letters 8 (2017) 3068–3072; doi:10.1021/acs.jpclett.7b01454

data_8000249
_publ_section_title
;
 Direct Observation of the Symmetrical and Asymmetrical Protonation States
 in Molecular Crystals.
;
_journal_issue                   13
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              3068
_journal_page_last               3072
_journal_paper_doi               10.1021/acs.jpclett.7b01454
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C28 H21 N2, Cl  2(H2 O)'
_chemical_formula_sum            'C28 H25 Cl N2 O2'
_chemical_formula_weight         456.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.70(3)
_cell_angle_beta                 88.68(3)
_cell_angle_gamma                66.35(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1571(16)
_cell_length_b                   9.862(2)
_cell_length_c                   15.677(3)
_cell_measurement_temperature    291(2)
_cell_volume                     1154.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9116
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4060
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+0.2194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2477
_reflns_number_gt                2461
_reflns_number_total             4060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz7b01454_si_003.cif
_cod_data_source_block           bp4va
_cod_depositor_comments
'Adding full bibliography for 8000248--8000249.cif.'
_cod_original_cell_volume        1154.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8000249