Thermal conversion of a pyridine solvate to a de-solvate facilitated by rearrangement of chalcogen bonds. The solvate and non-solvate structures of N-(2-nitro-4-(3-oxobenzo[d][1,2]selenazol-2(3H)-yl)phenyl)picolinamide
Fellowes, Thomas; van Koeverden, Martin P.; White, Jonathan; CrystEngComm  (2020) –; doi:10.1039/D0CE00662A

data_7240583
_publ_section_title
;
 Thermal conversion of a pyridine solvate to a de-solvate facilitated by
 rearrangement of chalcogen bonds. The solvate and non-solvate structures
 of N-(2-nitro-4-(3-oxobenzo[d][1,2]selenazol-2(3H)-yl)phenyl)picolinamide
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00662A
_journal_year                    2020
_chemical_formula_sum            'C24 H17 N5 O4 Se'
_chemical_formula_weight         518.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-05-02 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.154(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.9726(2)
_cell_length_b                   14.6836(5)
_cell_length_c                   14.4255(5)
_cell_measurement_reflns_used    3423
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4450
_cell_measurement_theta_min      3.0190
_cell_volume                     1042.64(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.36a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6794
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.785
_diffrn_reflns_theta_min         3.010
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.36a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       needle
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 848 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3132
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0561P)^2^+0.3921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.451
_reflns_Friedel_fraction_full    0.501
_reflns_Friedel_fraction_max     0.443
_reflns_number_gt                2977
_reflns_number_total             3132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00662a2.cif
_cod_data_source_block           1PYR
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7240583
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'Tom Fellowes Se intermediate with pyridine'
_oxdiff_exptl_absorpt_empirical_full_min 0.759
_oxdiff_exptl_absorpt_empirical_full_max 1.299
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              51376