A synthetic co-crystal prepared by cooperative single-crystal-to-single-crystal solid-state Diels-Alder reaction.
Khorasani, S.; Fernandes, M. A.; Chemical communications (Cambridge, England) 53 (2017) 4969–4972; doi:10.1039/c6cc07628a

data_7119951
_publ_section_title
;
 A synthetic co-crystal prepared by cooperative
 single-crystal-to-single-crystal solid-state Diels-Alder reaction.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4969
_journal_page_last               4972
_journal_paper_doi               10.1039/c6cc07628a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
;
0.34(C30 H23 Br N2 O4 S2), 0.66(C16 H14 N2 O4 S2), 1.66(C14 H9 Br)
;
_chemical_formula_sum            'C44 H32 Br2 N2 O4 S2'
_chemical_formula_weight         876.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-06 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                93.968(3)
_cell_angle_beta                 109.971(3)
_cell_angle_gamma                91.879(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6501(4)
_cell_length_b                   9.6910(4)
_cell_length_c                   11.4533(5)
_cell_measurement_reflns_used    8063
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.51
_cell_volume                     898.58(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0582
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10782
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    2.422
_exptl_absorpt_correction_T_max  0.8742
_exptl_absorpt_correction_T_min  0.5175
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Face indexed absorption corrections
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_recrystallization_method 'Thermal solid-state reacttion'
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.373
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         3159
_refine_ls_number_restraints     390
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+4.7605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2726
_reflns_number_total             3159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07628a2.cif
_cod_data_source_block           D4Br_2h
_cod_depositor_comments
'Adding full bibliography for 7119945--7119961.cif.'
_cod_database_code               7119951
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.378
_shelx_estimated_absorpt_t_max   0.797
_shelx_res_checksum              16477