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_7118581
_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            'C9 H10 B F4 N O2'
_chemical_formula_weight         250.99
_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                115.130(16)
_cell_angle_beta                 100.802(13)
_cell_angle_gamma                101.825(14)
_cell_formula_units_Z            2
_cell_length_a                   7.2802(11)
_cell_length_b                   9.0670(15)
_cell_length_c                   9.7329(16)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.5450
_cell_measurement_theta_min      3.0160
_cell_volume                     541.32(19)
_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
;
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 0.996
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_details
;
  1 omega  -33.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596   57.0000  -60.0000 85

  2 omega   -5.00   23.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596  -99.0000 -180.0000 28

  3 omega  -20.00   11.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596  -99.0000  -30.0000 31

  4 omega  -34.00   48.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596   57.0000   60.0000 82

  5 omega   -6.00   21.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596  -99.0000   60.0000 27

  6 omega  -85.00  -59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596 -179.0000 -150.0000 26

  7 omega  -85.00   -4.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3596  -57.0000  150.0000 81

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.1206
_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       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04297
_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    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1062P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2686
_reflns_number_gt                1092
_reflns_number_total             2441
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc09412g2.cif
_cod_data_source_block           1HBF4_2
_cod_original_cell_volume        541.32(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118581