#------------------------------------------------------------------------------
#$Date: 2023-09-18 10:37:01 +0300 (Mon, 18 Sep 2023) $
#$Revision: 286377 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/75/8107504.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_8107504
loop_
_publ_author_name
'Luo, Xinyao'
'Chen, Cuilian'
'Hu, Zunjian'
'Wang, Fei'
'Sun, Shanhu'
'Suo, Zhirong'
'Su, Li'
_publ_section_title
;
 Crystal structure of a polymorph of potassium picrate, C6H2KN3O7
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              593
_journal_page_last               594
_journal_paper_doi               10.1515/ncrs-2023-0068
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         '0.5(C12 H4 K2 N6 O14)'
_chemical_formula_sum            'C6 H2 K N3 O7'
_chemical_formula_weight         267.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 95.134(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.1681(2)
_cell_length_b                   10.6704(6)
_cell_length_c                   10.2381(6)
_cell_measurement_reflns_used    1522
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      3.82
_cell_volume                     453.52(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4245
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         2.763
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8669.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0404
_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/[σ²(Fo²)+(0.0412P)²+0.2069P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                764
_reflns_number_total             980
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0068_suppl_001.cif
_cod_data_source_block           16_0m
_cod_database_code               8107504
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
K1 K 1.04570(19) 0.2500 0.37078(8) 0.0405(3) Uani 1 2 d S T P . .
O1 O 0.6265(7) 0.2500 0.5494(2) 0.0505(7) Uani 1 2 d S T P . .
O3 O 0.4385(5) 0.57775(16) 0.72043(19) 0.0551(5) Uani 1 1 d . . . . .
O2 O 0.7861(5) 0.48793(17) 0.6097(2) 0.0576(6) Uani 1 1 d . . . . .
N1 N 0.5737(5) 0.48357(18) 0.6848(2) 0.0401(5) Uani 1 1 d . . . . .
O4 O 0.0489(6) 0.3505(2) 1.0772(2) 0.0779(7) Uani 1 1 d . . . . .
N2 N 0.1131(8) 0.2500 1.0284(3) 0.0527(9) Uani 1 2 d S T P . .
C1 C 0.5487(8) 0.2500 0.6636(3) 0.0339(7) Uani 1 2 d S T P . .
C2 C 0.4871(6) 0.3627(2) 0.7363(2) 0.0333(5) Uani 1 1 d . . . . .
C4 C 0.2692(8) 0.2500 0.9075(3) 0.0368(8) Uani 1 2 d S T P . .
C3 C 0.3435(6) 0.3634(2) 0.8519(2) 0.0372(6) Uani 1 1 d . . . . .
H3 H 0.2971 0.4386 0.8921 0.045 Uiso 1 1 calc R . . . .
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'
K K 0.2009 0.2494 '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
O1 K1 O1 97.48(8) . 1_655
O1 K1 O3 74.43(6) . 3_666
O1 K1 O3 74.43(6) . 2_646
O1 K1 O3 138.01(4) . 2_746
O1 K1 O3 67.67(5) 1_655 2_746
O1 K1 O3 138.01(4) . 3_766
O1 K1 O3 67.67(5) 1_655 3_766
O1 K1 O2 97.12(4) . 3_766
O1 K1 O2 97.12(4) . 2_746
O1 K1 N1 73.98(4) 1_655 3_766
O1 K1 N1 118.26(4) . 2_746
O1 K1 N1 118.26(4) . 3_766
O1 K1 N1 73.98(4) 1_655 2_746
O1 K1 O4 135.32(8) . 4_664
O1 K1 O4 121.33(7) 1_655 1_654
O1 K1 O4 135.32(7) . 1_654
O1 K1 O4 121.33(7) 1_655 4_664
O3 K1 O1 137.69(4) 3_666 1_655
O3 K1 O1 137.69(4) 2_646 1_655
O3 K1 O3 90.52(5) 2_646 2_746
O3 K1 O3 142.74(8) 2_646 3_766
O3 K1 O3 142.74(8) 3_666 2_746
O3 K1 O3 90.52(5) 3_666 3_766
O3 K1 O3 81.14(8) 2_646 3_666
O3 K1 O3 74.45(7) 3_766 2_746
O3 K1 O2 144.59(6) 3_666 2_746
O3 K1 O2 63.54(6) 2_646 2_746
O3 K1 O2 144.59(6) 2_646 3_766
O3 K1 O2 63.54(6) 3_666 3_766
O3 K1 N1 146.72(6) 3_666 2_746
O3 K1 N1 21.54(5) 3_766 3_766
O3 K1 N1 74.06(5) 2_646 2_746
O3 K1 N1 95.91(5) 3_766 2_746
O3 K1 N1 95.91(5) 2_746 3_766
O3 K1 N1 146.72(6) 2_646 3_766
O3 K1 N1 74.06(5) 3_666 3_766
O3 K1 N1 21.54(5) 2_746 2_746
O3 K1 O4 88.31(6) 2_646 1_654
O3 K1 O4 88.31(6) 3_666 4_664
O3 K1 O4 81.44(6) 3_766 4_664
O3 K1 O4 62.19(6) 2_646 4_664
O3 K1 O4 56.26(6) 2_746 4_664
O3 K1 O4 62.19(6) 3_666 1_654
O3 K1 O4 56.26(6) 3_766 1_654
O3 K1 O4 81.44(6) 2_746 1_654
O2 K1 O1 76.85(5) 2_746 1_655
O2 K1 O1 76.85(5) 3_766 1_655
O2 K1 O3 115.68(5) 3_766 2_746
O2 K1 O3 42.34(5) 3_766 3_766
O2 K1 O3 42.34(5) 2_746 2_746
O2 K1 O3 115.68(5) 2_746 3_766
O2 K1 O2 151.45(9) 3_766 2_746
O2 K1 N1 136.29(6) 3_766 2_746
O2 K1 N1 21.21(5) 2_746 2_746
O2 K1 N1 136.29(6) 2_746 3_766
O2 K1 N1 21.21(5) 3_766 3_766
O2 K1 O4 73.62(6) 3_766 1_654
O2 K1 O4 111.67(6) 3_766 4_664
O2 K1 O4 111.67(6) 2_746 1_654
O2 K1 O4 73.62(6) 2_746 4_664
N1 K1 N1 117.27(7) 3_766 2_746
O4 K1 N1 94.81(6) 1_654 2_746
O4 K1 N1 60.65(6) 4_664 2_746
O4 K1 N1 94.81(6) 4_664 3_766
O4 K1 N1 60.65(6) 1_654 3_766
O4 K1 O4 39.27(8) 4_664 1_654
K1 O1 K1 97.48(8) . 1_455
C1 O1 K1 108.7(2) . 1_455
C1 O1 K1 153.9(2) . .
K1 O3 K1 90.52(5) 3_666 3_766
N1 O3 K1 140.35(16) . 3_666
N1 O3 K1 92.75(14) . 3_766
N1 O2 K1 100.27(14) . 3_766
O3 N1 K1 65.72(12) . 3_766
O3 N1 C2 119.05(19) . .
O2 N1 K1 58.52(12) . 3_766
O2 N1 O3 122.28(19) . .
O2 N1 C2 118.63(19) . .
C2 N1 K1 163.51(16) . 3_766
N2 O4 K1 96.29(18) . 1_456
O4 N2 O4 122.6(3) 4_565 .
O4 N2 C4 118.71(16) . .
O4 N2 C4 118.72(16) 4_565 .
O1 C1 K1 51.72(19) . 1_455
O1 C1 C2 123.88(13) . 4_565
O1 C1 C2 123.88(13) . .
C2 C1 K1 108.66(18) . 1_455
C2 C1 K1 108.66(18) 4_565 1_455
C2 C1 C2 112.1(3) . 4_565
N1 C2 C1 119.3(2) . .
C3 C2 N1 116.73(19) . .
C3 C2 C1 124.0(2) . .
C3 C4 N2 119.05(15) . .
C3 C4 N2 119.05(15) 4_565 .
C3 C4 C3 121.9(3) . 4_565
C2 C3 C4 118.7(2) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.640(2) .
K1 O1 2.900(3) 1_655
K1 O3 3.038(2) 3_766
K1 O3 2.826(2) 2_646
K1 O3 2.826(2) 3_666
K1 O3 3.038(2) 2_746
K1 O2 2.8855(18) 2_746
K1 O2 2.8855(18) 3_766
K1 N1 3.3293(19) 2_746
K1 N1 3.3293(19) 3_766
K1 O4 3.193(2) 4_664
K1 O4 3.193(2) 1_654
O1 K1 2.900(3) 1_455
O1 C1 1.241(4) .
O3 K1 3.038(2) 3_766
O3 K1 2.826(2) 3_666
O3 N1 1.224(2) .
O2 K1 2.8855(18) 3_766
O2 N1 1.224(2) .
N1 K1 3.3293(19) 3_766
N1 C2 1.451(3) .
O4 K1 3.193(2) 1_456
O4 N2 1.223(2) .
N2 O4 1.223(2) 4_565
N2 C4 1.448(4) .
C1 K1 3.501(4) 1_455
C1 C2 1.449(3) 4_565
C1 C2 1.449(3) .
C2 C3 1.373(3) .
C4 C3 1.384(3) .
C4 C3 1.384(3) 4_565
C3 H3 0.9300 .
