A single-crystal-to-single-crystal Diels‒Alder reaction with mixed topochemical and topotactic behaviour
Khorasani, S.; Botes, D. S.; Fernandes, M. A.; Levendis, D. C.; CrystEngComm 17 (2015) 8933–; doi:10.1039/C5CE01301A

data_7222090
_publ_section_title
;
 A single-crystal-to-single-crystal Diels--Alder reaction with mixed
 topochemical and topotactic behaviour
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8933
_journal_paper_doi               10.1039/C5CE01301A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'0.581(C28 H19 Br N2 O4 S2), 0.419(C14 H10 N2 O4 S2), 0.419(C14 H9 Br)'
_chemical_formula_sum            'C28 H19 Br N2 O4 S2'
_chemical_formula_weight         591.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-07 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.180(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.905(2)
_cell_length_b                   14.015(2)
_cell_length_c                   14.524(3)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.91
_cell_volume                     2481.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2648
_diffrn_reflns_av_unetI/netI     0.1160
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            96915
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.890
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  0.9012
_exptl_absorpt_correction_T_min  0.6214
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'Face indexed absorption corrections carried out with XPREP'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Thermal solid-state reaction from CT crystal'
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.871
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 1466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.499(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         8691
_refine_ls_number_restraints     1534
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.2358
_refine_ls_R_factor_gt           0.1463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1639P)^2^+37.1995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3412
_refine_ls_wR_factor_ref         0.4108
_reflns_Friedel_coverage         0.908
_reflns_friedel_fraction_full    0.991
_reflns_friedel_fraction_max     0.991
_reflns_number_gt                4787
_reflns_number_total             8691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01301a1.cif
_cod_data_source_block           31days_reaction_p21_refine
_cod_depositor_comments
'Adding full bibliography for 7222085--7222099.cif.'
_cod_original_cell_volume        2481.1(7)
_cod_database_code               7222090
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.474
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              64729