The crystal structure of 5-nitropicolinic acid monohydrate, C6H6N2O5
Jia, Hua-Li; Wang, Xin; Dai, Li-Yan; Wang, Li-Ke; Ren, Xiao-Yue; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 733–734; doi:10.1515/ncrs-2019-0934

data_8105272
_publ_section_title
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 The crystal structure of 5-nitropicolinic acid monohydrate, C6H6N2O5
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              733
_journal_page_last               734
_journal_paper_doi               10.1515/ncrs-2019-0934
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C6 H4 N2 O4, H2 O'
_chemical_formula_sum            'C6 H6 N2 O5'
_chemical_formula_weight         186.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.081(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1766(11)
_cell_length_b                   5.1019(4)
_cell_length_c                   22.602(2)
_cell_measurement_reflns_used    3400
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      3.09
_cell_volume                     1519.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015) [1]'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [4]'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015) [3]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015) [2]'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device       'Bruker APEX-II diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9766
_diffrn_reflns_theta_full        25.1732
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         3.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0700 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.4094.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.6274
_exptl_crystal_description       block
_exptl_crystal_F_000             768.5832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.1941
_refine_diff_density_min         -0.2011
_refine_diff_density_rms         0.0513
_refine_ls_d_res_high            0.8355
_refine_ls_d_res_low             6.5871
_refine_ls_goodness_of_fit_ref   1.0680
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0680
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.5678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                1107
_reflns_number_total             1366
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2019-0934_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               8105272
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1Wa,H1Wb)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
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_olex2_submission_special_instructions 'No special instructions were received'