Three peroxomorphic H2O2 adducts of antibiotic furacin: the first cases of 2D hydrogen-bonded peroxide layers and concerted flip-flop hydrogen disorder of peroxide species
Churakov, Andrei V.; CrystEngComm 26 (2024) 5996–6002; doi:10.1039/D4CE00822G

data_7249412
_publ_section_title
;
 Three peroxomorphic H2O2 adducts of antibiotic furacin: the first cases
 of 2D hydrogen-bonded peroxide layers and concerted flip-flop hydrogen
 disorder of peroxide species
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5996
_journal_page_last               6002
_journal_paper_doi               10.1039/D4CE00822G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(C6 H6 N4 O4), 7(H2 O2)'
_chemical_formula_sum            'C12 H26 N8 O22'
_chemical_formula_weight         634.41
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-04 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                105.6813(13)
_cell_angle_beta                 108.5010(13)
_cell_angle_gamma                103.7032(14)
_cell_formula_units_Z            2
_cell_length_a                   8.8432(3)
_cell_length_b                   12.7456(5)
_cell_length_c                   13.2427(5)
_cell_measurement_reflns_used    7300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.531
_cell_measurement_theta_min      2.576
_cell_volume                     1274.85(9)
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.9281
_exptl_transmission_factor_min   0.8807
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6764
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0463P)^2^+0.6905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5311
_reflns_number_total             6764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00822g3.cif
_cod_data_source_block           d
_cod_depositor_comments
'Adding full bibliography for 7249410--7249412.cif.'
_cod_original_cell_volume        1274.85(8)
_cod_database_code               7249412
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              67327
_shelx_hkl_checksum              62575