Solvation and oxidation effects on the crystal structure and morphology of tetraoxolene-based materials
Kamin, Ashlyn A.; Brannan, E. J.; Snook, Kathleen M.; Krajewski, Sebastian; Gannon, Paige M.; Kaminsky, Werner; Xiao, Dianne J.; CrystEngComm 26 (2024) 6396–6402; doi:10.1039/D4CE00921E

data_7249512
_publ_section_title
;
 Solvation and oxidation effects on the crystal structure and morphology
 of tetraoxolene-based materials
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              6396
_journal_page_last               6402
_journal_paper_doi               10.1039/D4CE00921E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C18 H10 Mn O4, 2(C4 H9 N O)'
_chemical_formula_sum            'C26 H28 Mn N2 O6'
_chemical_formula_weight         519.44
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2021-08-11T12:08:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-09-10 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.241(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0608(9)
_cell_length_b                   13.3977(14)
_cell_length_c                   11.7569(14)
_cell_measurement_reflns_used    3092
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.36
_cell_measurement_theta_min      2.3
_cell_measurement_wavelength     0.71073
_cell_volume                     1269.4(2)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.06327
_diffrn_orient_matrix_UB_12      -0.071848
_diffrn_orient_matrix_UB_13      0.006592
_diffrn_orient_matrix_UB_21      0.084524
_diffrn_orient_matrix_UB_22      0.040716
_diffrn_orient_matrix_UB_23      0.042297
_diffrn_orient_matrix_UB_31      -0.065192
_diffrn_orient_matrix_UB_32      -0.020449
_diffrn_orient_matrix_UB_33      0.061144
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 1
_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       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9415
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.853
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             542
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylacetamide/methanol'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0
_reflns_number_gt                1757
_reflns_number_total             3018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00921e2.cif
_cod_data_source_block           trans-Mn(Ph2dhbq)(DMA)2
_cod_depositor_comments
'Adding full bibliography for 7249512--7249515.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7249512
_shelx_estimated_absorpt_t_min   0.93
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              40689