Single crystal to single crystal [2+2] photoreactions in chloride and sulphate salts of 4-amino-cinnamic acid via solid-solution formation: a structural and kinetic study.
d'Agostino, Simone; Spinelli, Floriana; Boanini, Elisa; Braga, Dario; Grepioni, Fabrizia; Chemical communications (Cambridge, England) 52 (2016) 1899–1902; doi:10.1039/c5cc09412g

data_7118573
_publ_section_title
;
 Single crystal to single crystal [2+2] photoreactions in chloride and
 sulphate salts of 4-amino-cinnamic acid via solid-solution formation: a
 structural and kinetic study.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1899
_journal_page_last               1902
_journal_paper_doi               10.1039/c5cc09412g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C18 H22 N2 O9 S'
_chemical_formula_weight         442.44
_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
_audit_update_record
;
2015-11-12 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                103.793(10)
_cell_angle_beta                 99.924(9)
_cell_angle_gamma                102.838(10)
_cell_formula_units_Z            2
_cell_length_a                   7.3374(8)
_cell_length_b                   10.5566(12)
_cell_length_c                   13.8798(15)
_cell_measurement_reflns_used    1642
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.4020
_cell_measurement_theta_min      3.4000
_cell_volume                     988.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2005)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_details
;
  1 omega  -25.00   17.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      -16.5159  -99.0000   30.0000 42

  2 omega  -12.00   24.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      -16.5159  -99.0000  120.0000 36

  3 omega   39.00   91.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -       17.7659 -179.0000   90.0000 52

  4 omega   10.00   58.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -       17.7659  -99.0000  -90.0000 48

  5 omega  -49.00   20.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -       17.7659  -57.0000  120.0000 69

  6 omega  -53.00   72.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -       17.7659    0.0000  150.0000 125

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8036
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.97150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0517P)^2^+0.8044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                2801
_reflns_number_total             4494
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc09412g2.cif
_cod_data_source_block           1H2SO4-H2O_2
_cod_original_cell_volume        988.76(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118573