Non-covalent interactions of hydroperoxo group in crystalline adducts of organic hydroperoxides and their potassium salts
Buldashov, Ivan A.; Medvedev, Alexander G.; Mikhaylov, Alexey A.; Andrei, Churakov; Lev, Ovadia; Prikhodchenko, Petr V.; CrystEngComm  (2022) –; doi:10.1039/D2CE01017H

data_7245298
_publ_section_title
;
 Non-covalent interactions of hydroperoxo group in crystalline adducts of
 organic hydroperoxides and their potassium salts
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01017H
_journal_year                    2022
_chemical_formula_moiety         'C6 H12 O4, C6 H11 O4, K'
_chemical_formula_sum            'C12 H23 K O8'
_chemical_formula_weight         334.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.9888(10)
_cell_length_b                   6.3547(3)
_cell_length_c                   9.8148(4)
_cell_measurement_reflns_used    8894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      3.261
_cell_volume                     1558.55(12)
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16054
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.993
_diffrn_reflns_theta_min         3.261
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.8345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2018)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0380P)^2^+3.9711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2057
_reflns_number_total             2258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01017h2.cif
_cod_data_source_block           a_CCDC1
_cod_database_code               7245298
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.864
_shelx_res_checksum              99323
_shelx_hkl_checksum              21747