#------------------------------------------------------------------------------
#$Date: 2026-03-05 13:43:27 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304900 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/15/7251552.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7251552
loop_
_publ_author_name
'Churakov, Andrei V.'
'Mel'nik, Elena A.'
'Egorov, Pavel A.'
'Mikhaylov, Alexey A.'
'Tripol'skaya, Tatiana A.'
'Lev, Ovadia'
'Prikhodchenko, Petr V.'
_publ_section_title
;
 Anion-directed architectures in amine halide peroxosolvates: role of
 H2O2/H2O competition in crystal engineering
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1225
_journal_page_last               1237
_journal_paper_doi               10.1039/D5CE01038A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C4 H12 N2, 2(H2 O2), 2(Cl)'
_chemical_formula_sum            'C4 H16 Cl2 N2 O4'
_chemical_formula_weight         227.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2025-06-01 deposited with the CCDC.	2025-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.808(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3636(4)
_cell_length_b                   11.0879(6)
_cell_length_c                   6.0534(3)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.469
_cell_measurement_theta_min      3.356
_cell_volume                     487.02(4)
_computing_cell_refinement       'SAINT (Bruker, 2018)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5409
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_min         3.355
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       prism
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0244P)²+0.1194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1175
_reflns_number_total             1287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce01038a2.cif
_cod_data_source_block           a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7251547--7251557.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7251552
_shelx_shelxl_version_number     2019/2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_file
;
TITL a in P2(1)/c
    a.res
    created by SHELXL-2019/2 at 18:52:25 on 16-Dec-2022
CELL 0.71073 7.3636 11.0879 6.0534 90 99.808 90
ZERR 2 0.0004 0.0006 0.0003 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N O
UNIT 8 32 4 4 8

EQIV $1 1-X,1-Y,1-Z
EQIV $2 1-X,1-Y,-Z

L.S. 10
PLAN  5
SIZE 0.1 0.05 0.05
TEMP -173
CONF
CONF H1 O1 O2 H2
HTAB O1 Cl1
HTAB O2 Cl1_$2
HTAB N1 Cl1_$2
HTAB N1 Cl1_$1
BOND $H
fmap 2 53
acta
OMIT -2 58
OMIT 1 0 0

WGHT    0.024400    0.119400
FVAR       1.71090
CL1   3    0.250974    0.365907    0.113032    11.00000    0.01399    0.00988 =
         0.00863    0.00011    0.00366   -0.00016
O1    5    0.456127    0.604530    0.254808    11.00000    0.01350    0.01472 =
         0.01430    0.00219   -0.00029   -0.00182
H1    2    0.401240    0.541510    0.205359    11.00000    0.03221
O2    5    0.377148    0.692432    0.085514    11.00000    0.01334    0.01449 =
         0.01982    0.00421    0.00193    0.00344
H2    2    0.460311    0.698889    0.011716    11.00000    0.03175
N1    4    0.852556    0.580290    0.409787    11.00000    0.00888    0.00808 =
         0.00847    0.00017    0.00135    0.00085
H3    2    0.812498    0.605509    0.528538    11.00000    0.01732
H4    2    0.788211    0.615365    0.287369    11.00000    0.02225
C1    1    0.830379    0.446695    0.385366    11.00000    0.00967    0.00806 =
         0.01076   -0.00066   -0.00013   -0.00069
H11   2    0.864538    0.427666    0.242686    11.00000    0.01261
H12   2    0.702278    0.425576    0.387260    11.00000    0.01429
C2    1    1.049160    0.617090    0.422597    11.00000    0.00839    0.00866 =
         0.01224    0.00189    0.00154    0.00017
H21   2    1.081077    0.596438    0.280776    11.00000    0.00991
H22   2    1.056865    0.705259    0.441994    11.00000    0.01533
HKLF 4




REM  a in P2(1)/c
REM wR2 = 0.0502, GooF = S = 1.059, Restrained GooF = 1.059 for all data
REM R1 = 0.0197 for 1175 Fo > 4sig(Fo) and 0.0226 for all 1287 data
REM 87 parameters refined using 0 restraints

END

WGHT      0.0244      0.1194

REM Highest difference peak  0.446,  deepest hole -0.215,  1-sigma level  0.046
Q1    1   0.8922  0.4187  0.4827  11.00000  0.05    0.45
Q2    1   0.8458  0.5127  0.4095  11.00000  0.05    0.33
Q3    1   0.9573  0.5984  0.4208  11.00000  0.05    0.26
Q4    1   1.0853  0.5819  0.3509  11.00000  0.05    0.15
Q5    1   1.0551  0.6627  0.4472  11.00000  0.05    0.15
;
_shelx_res_checksum              9728
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.25097(3) 0.36591(2) 0.11303(3) 0.01063(8) Uani 1 1 d . . . . .
O1 O 0.45613(10) 0.60453(7) 0.25481(12) 0.01448(16) Uani 1 1 d . . . . .
H1 H 0.401(2) 0.5415(14) 0.205(3) 0.032(4) Uiso 1 1 d . . . . .
O2 O 0.37715(10) 0.69243(7) 0.08551(13) 0.01599(16) Uani 1 1 d . . . . .
H2 H 0.460(2) 0.6989(13) 0.012(3) 0.032(4) Uiso 1 1 d . . . . .
N1 N 0.85256(11) 0.58029(7) 0.40979(13) 0.00849(16) Uani 1 1 d . . . . .
H3 H 0.8125(19) 0.6055(12) 0.529(2) 0.017(3) Uiso 1 1 d . . . . .
H4 H 0.788(2) 0.6154(12) 0.287(2) 0.022(3) Uiso 1 1 d . . . . .
C1 C 0.83038(13) 0.44669(8) 0.38537(16) 0.00971(18) Uani 1 1 d . . . . .
H11 H 0.8645(17) 0.4277(11) 0.243(2) 0.013(3) Uiso 1 1 d . . . . .
H12 H 0.7023(18) 0.4256(12) 0.387(2) 0.014(3) Uiso 1 1 d . . . . .
C2 C 1.04916(13) 0.61709(8) 0.42260(16) 0.00979(18) Uani 1 1 d . . . . .
H21 H 1.0811(17) 0.5964(10) 0.281(2) 0.010(3) Uiso 1 1 d . . . . .
H22 H 1.0569(17) 0.7053(11) 0.442(2) 0.015(3) Uiso 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.01399(13) 0.00988(11) 0.00863(11) 0.00011(8) 0.00366(8) -0.00016(8)
O1 0.0135(4) 0.0147(3) 0.0143(4) 0.0022(3) -0.0003(3) -0.0018(3)
O2 0.0133(4) 0.0145(3) 0.0198(4) 0.0042(3) 0.0019(3) 0.0034(3)
N1 0.0089(4) 0.0081(3) 0.0085(4) 0.0002(3) 0.0014(3) 0.0009(3)
C1 0.0097(4) 0.0081(4) 0.0108(4) -0.0007(3) -0.0001(3) -0.0007(3)
C2 0.0084(4) 0.0087(4) 0.0122(4) 0.0019(3) 0.0015(3) 0.0002(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 O1 H1 101.3(10) . . ?
O1 O2 H2 101.3(11) . . ?
C2 N1 C1 111.38(7) . . ?
C2 N1 H3 109.4(9) . . ?
C1 N1 H3 110.7(9) . . ?
C2 N1 H4 107.2(9) . . ?
C1 N1 H4 108.3(9) . . ?
H3 N1 H4 109.8(13) . . ?
N1 C1 C2 110.33(8) . 3_766 ?
N1 C1 H11 105.4(7) . . ?
C2 C1 H11 112.2(8) 3_766 . ?
N1 C1 H12 109.1(8) . . ?
C2 C1 H12 108.7(7) 3_766 . ?
H11 C1 H12 111.1(10) . . ?
N1 C2 C1 110.40(7) . 3_766 ?
N1 C2 H21 105.8(7) . . ?
C1 C2 H21 112.1(7) 3_766 . ?
N1 C2 H22 108.2(7) . . ?
C1 C2 H22 111.0(7) 3_766 . ?
H21 C2 H22 109.1(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 O2 1.4613(10) . ?
O1 H1 0.837(16) . ?
O2 H2 0.820(16) . ?
N1 C2 1.4934(12) . ?
N1 C1 1.4948(12) . ?
N1 H3 0.868(14) . ?
N1 H4 0.897(15) . ?
C1 C2 1.5123(13) 3_766 ?
C1 H11 0.963(12) . ?
C1 H12 0.974(13) . ?
C2 H21 0.956(12) . ?
C2 H22 0.985(12) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 Cl1 0.837(16) 2.262(16) 3.0947(8) 173.4(14) . yes
O2 H2 Cl1 0.820(16) 2.481(16) 3.2377(8) 154.0(14) 3_665 yes
N1 H4 Cl1 0.897(15) 2.401(15) 3.1830(8) 145.8(12) 3_665 yes
N1 H3 Cl1 0.868(14) 2.318(14) 3.1672(8) 165.9(12) 3_666 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 C2 57.02(11) . . . 3_766 ?
C1 N1 C2 C1 -57.06(11) . . . 3_766 ?
H1 O1 O2 H2 -102.0(15) . . . . ?
