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_7249513
_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_absolute_configuration unk
_chemical_formula_moiety         'C24 H24 Mn N2 O6'
_chemical_formula_sum            'C24 H24 Mn N2 O6'
_chemical_formula_weight         491.39
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      144
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_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             2022-05-26T10:25:18-00:00
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.1118(12)
_cell_length_b                   10.1118(12)
_cell_length_c                   18.832(3)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      3.2
_cell_volume                     1667.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.96
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31856
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         26.831
_diffrn_reflns_theta_min         2.218
_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    0.677
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             765
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylformamide/methanol'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4271
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0638P)^2^+0.2085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         1
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                4056
_reflns_number_total             4271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00921e2.cif
_cod_data_source_block           cis-Mn(Ph2dhbq)(DMF)2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7249512--7249515.cif.
;
_cod_original_cell_volume        1667.6(5)
_cod_database_code               7249513
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.987
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              27482