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_8000248
_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 H22 N2, S O4, 2(H2 O)'
_chemical_formula_sum            'C28 H26 N2 O6 S'
_chemical_formula_weight         518.57
_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                83.45(3)
_cell_angle_beta                 77.59(3)
_cell_angle_gamma                85.73(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3018(17)
_cell_length_b                   9.4214(19)
_cell_length_c                   16.293(3)
_cell_measurement_reflns_used    6896
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.06
_cell_volume                     1234.8(5)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scans'
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.1408
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12125
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9086
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5590
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0654P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                2823
_reflns_number_total             5590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz7b01454_si_004.cif
_cod_data_source_block           BP4VA-2H
_cod_depositor_comments
'Adding full bibliography for 8000248--8000249.cif.'
_cod_original_cell_volume        1234.8(4)
_cod_database_code               8000248