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#$Date: 2022-05-09 12:10:04 +0300 (Mon, 09 May 2022) $
#$Revision: 275277 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/51/8105190.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_8105190
loop_
_publ_author_name
'Cong, Chen'
'Yun, Xiao'
'Chong, Li'
'LiZhen, Chen'
'Jianlong, Wang'
_publ_section_title
;
 The crystal structure of 1-methyl-1H-pyrazol-2-ium nitrate, C4H7O3N3
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              237
_journal_page_last               238
_journal_paper_doi               10.1515/ncrs-2021-0474
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'N O3, 0.5(C8 H14 N4)'
_chemical_formula_sum            'C4 H7 N3 O3'
_chemical_formula_weight         145.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2289(10)
_cell_length_b                   6.1881(4)
_cell_length_c                   7.5592(5)
_cell_measurement_reflns_used    1247
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.077
_cell_measurement_theta_min      2.863
_cell_volume                     665.59(8)
_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      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3531
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.355
_diffrn_reflns_theta_min         2.863
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0967 before and 0.0403 after correction. The Ratio of minimum to maximum transmission is 0.8477. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0427
_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)+(0.0449P)²+0.2821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                585
_reflns_number_total             737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0474_suppl.cif
_cod_data_source_block           c
_cod_database_code               8105190
_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_max   0.994
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2
 0.87 with sigma of 0.02
3. Others
 Fixed Sof: H1C(0.5) H1B(0.5) H1A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4)
4.b Idealised Me refined as rotating group:
 C1(H1C,H1B,H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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
O1 O 0.55042(10) 0.250000 0.5349(2) 0.0363(5) Uani 1 2 d S T P . .
O2 O 0.65501(11) 0.250000 0.3276(2) 0.0419(5) Uani 1 2 d S T P . .
O3 O 0.50675(14) 0.250000 0.2602(2) 0.0463(6) Uani 1 2 d S T P . .
N2 N 0.36760(13) 0.250000 0.5856(2) 0.0273(5) Uani 1 2 d DS T P . .
N1 N 0.33810(13) 0.250000 0.7545(2) 0.0276(5) Uani 1 2 d S T P . .
N3 N 0.57104(13) 0.250000 0.3713(3) 0.0303(5) Uani 1 2 d S T P . .
C2 C 0.24443(17) 0.250000 0.7564(4) 0.0359(7) Uani 1 2 d S T P . .
H2A H 0.205788 0.250000 0.858919 0.043 Uiso 1 2 calc RS T P . .
C3 C 0.21338(16) 0.250000 0.5833(4) 0.0385(7) Uani 1 2 d S T P . .
H3 H 0.150044 0.250000 0.543535 0.046 Uiso 1 2 calc RS T P . .
C4 C 0.29281(16) 0.250000 0.4807(3) 0.0339(6) Uani 1 2 d S T P . .
H4 H 0.294106 0.250000 0.355042 0.041 Uiso 1 2 calc RS T P . .
C1 C 0.40502(19) 0.250000 0.8999(3) 0.0410(7) Uani 1 2 d S T P . .
H1C H 0.372162 0.282803 1.010671 0.062 Uiso 0.5 1 calc GR . . A -1
H1B H 0.453335 0.359746 0.878360 0.062 Uiso 0.5 1 calc GR . . A -1
H1A H 0.434655 0.107450 0.908807 0.062 Uiso 0.5 1 calc GR . . A -1
H2 H 0.4313(14) 0.250000 0.551(4) 0.084(12) Uiso 1 2 d DS T P . .
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'
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
C4 N2 N1 108.49(19) . .
N2 N1 C1 120.91(19) . .
C2 N1 N2 108.8(2) . .
C2 N1 C1 130.3(2) . .
O2 N3 O1 118.80(19) . .
O2 N3 O3 122.0(2) . .
O3 N3 O1 119.21(19) . .
N1 C2 C3 108.0(2) . .
C4 C3 C2 105.8(2) . .
N2 C4 C3 108.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 N3 1.271(3) .
O2 N3 1.240(2) .
O3 N3 1.242(2) .
N2 N1 1.344(3) .
N2 C4 1.327(3) .
N1 C2 1.333(3) .
N1 C1 1.455(3) .
C2 C3 1.381(4) .
C3 C4 1.371(3) .
