Coordination vs. oxidative rearrangement of photochromic spiropyrans upon reacting with FeIIICl3 and FeIIIBr3
Osipov, Nikita G.; Faraonov, Maxim A.; Kuzmin, Alexey V.; Khasanov, Salavat S.; Shestakov, Alexander F.; Denisov, Nikolay N.; Savinykh, Tatiana A.; Otsuka, Akihiro; Kitagawa, Hiroshi; Konarev, Dmitri V.; New Journal of Chemistry 48 (2024) 13526–13537; doi:10.1039/D4NJ02371D

data_7063328
_publ_section_title
;
 Coordination vs. oxidative rearrangement of photochromic spiropyrans upon
 reacting with FeIIICl3 and FeIIIBr3
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13526
_journal_page_last               13537
_journal_paper_doi               10.1039/D4NJ02371D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         '2(C22 H20 N2 O Fe Br3), C6 H4 Cl2'
_chemical_formula_sum            'C50 H44 Br6 Cl2 Fe2 N4 O2'
_chemical_formula_weight         1394.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2024-03-26 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                94.350(9)
_cell_angle_beta                 94.322(10)
_cell_angle_gamma                92.784(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4022(11)
_cell_length_b                   12.9570(15)
_cell_length_c                   24.221(3)
_cell_measurement_reflns_used    3268
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      28.9060
_cell_measurement_theta_min      3.2570
_cell_volume                     2617.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      155(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.753
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_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  0.0941
_diffrn_reflns_av_unetI/netI     0.1926
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.753
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18722
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.753
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.456
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.278
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         10948
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      0.831
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0642P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4801
_reflns_number_total             10948
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 2.0977\% 
 around [-0.48 -0.77 -0.42] (reciprocal) or [-0.83 -0.55 -0.12] (direct)
;
_cod_data_source_file            d4nj02371d2.cif
_cod_data_source_block           PhotoN-FeBr3
_cod_depositor_comments
'Adding full bibliography for 7063326--7063329.cif.'
_cod_original_cell_volume        2617.9(5)
_cod_database_code               7063328
_shelx_estimated_absorpt_t_min   0.386
_shelx_estimated_absorpt_t_max   0.736
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelxl_version_number           2013-2
_shelx_res_checksum              73659
_shelx_hkl_checksum              44490