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_7249515
_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         'C72 H72 N6 Nd2 O18, 4(C3 H7 N O), H2 O'
_chemical_formula_sum            'C84 H102 N10 Nd2 O23'
_chemical_formula_weight         1908.23
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_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             2024-01-10T14:37:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-09-11 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                81.48(2)
_cell_angle_beta                 88.19(2)
_cell_angle_gamma                69.49(2)
_cell_formula_units_Z            2
_cell_length_a                   12.033(6)
_cell_length_b                   14.668(7)
_cell_length_c                   27.099(12)
_cell_measurement_reflns_used    8434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.38
_cell_measurement_wavelength     0.7288
_cell_volume                     4429(4)
_computing_cell_refinement       'SAINT V8.38A 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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON II CPAD detector'
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.085003
_diffrn_orient_matrix_UB_12      -0.01069
_diffrn_orient_matrix_UB_13      0.007966
_diffrn_orient_matrix_UB_21      -0.018451
_diffrn_orient_matrix_UB_22      0.072753
_diffrn_orient_matrix_UB_23      -0.005832
_diffrn_orient_matrix_UB_31      -0.017973
_diffrn_orient_matrix_UB_32      0.003181
_diffrn_orient_matrix_UB_33      0.036181
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57327
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         27.097
_diffrn_reflns_theta_min         0.779
_diffrn_source                   'ALS-U Lawrence Berkeley National Laboratory'
_diffrn_source_type              'ALS-U Beamline 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2016/2 - Bruker AXS area detector scaling and absorption correcti
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylformamide'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.188
_refine_diff_density_min         -2.623
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         16406
_refine_ls_number_restraints     835
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+180.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2547
_reflns_Friedel_coverage         0
_reflns_number_gt                11076
_reflns_number_total             16406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00921e2.cif
_cod_data_source_block           Nd2(Ph2dhbq)3(DMF)6
_cod_depositor_comments
'Adding full bibliography for 7249512--7249515.cif.'
_cod_database_code               7249515
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.974
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              51505