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_7249514
_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         'C27 H31 N4 Nd O10'
_chemical_formula_sum            'C27 H31 N4 Nd O10'
_chemical_formula_weight         715.8
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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      2.4.5
_audit_creation_date             2023-06-05T12:24:44-00:00
_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                93.854(8)
_cell_angle_beta                 113.574(8)
_cell_angle_gamma                91.387(8)
_cell_formula_units_Z            2
_cell_length_a                   10.4589(17)
_cell_length_b                   12.0484(19)
_cell_length_c                   12.740(2)
_cell_measurement_reflns_used    9629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.78
_cell_measurement_theta_min      2.33
_cell_measurement_wavelength     0.71073
_cell_volume                     1465.8(4)
_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-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_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      0.103767
_diffrn_orient_matrix_UB_12      -0.000739
_diffrn_orient_matrix_UB_13      0.041661
_diffrn_orient_matrix_UB_21      0.004949
_diffrn_orient_matrix_UB_22      -0.044639
_diffrn_orient_matrix_UB_23      -0.067212
_diffrn_orient_matrix_UB_31      0.011145
_diffrn_orient_matrix_UB_32      0.070345
_diffrn_orient_matrix_UB_33      -0.033669
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.029
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            84305
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.805
_diffrn_reflns_theta_min         1.697
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2012/1 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             722
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylformamide'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     390
_refine_ls_number_reflns         11769
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+0.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0
_reflns_number_gt                11087
_reflns_number_total             11769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00921e2.cif
_cod_data_source_block           Nd(Ph2dhbq)2(DMF)3(NO3)
_cod_depositor_comments
'Adding full bibliography for 7249512--7249515.cif.'
_cod_database_code               7249514
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.947
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              28626