Crystal structure of (E)-2-((2-(pyrimidin-2-yl)hydrazono)methyl)quinolin-1-ium perchlorate – methanol (1/1), C15H16N5O5Cl
Yang, Huanhuan; Shi, Fanyu; Xu, Qingqing; Wang, Jinghai; Xing, Ai-Ping; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 635–637; doi:10.1515/ncrs-2019-0873

data_8105242
_publ_section_title
;
 Crystal structure of
 (E)-2-((2-(pyrimidin-2-yl)hydrazono)methyl)quinolin-1-ium perchlorate --
 methanol (1/1), C15H16N5O5Cl
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              635
_journal_page_last               637
_journal_paper_doi               10.1515/ncrs-2019-0873
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'Cl O4, C H4 O, C14 H12 N5'
_chemical_formula_sum            'C15 H16 Cl N5 O5'
_chemical_formula_weight         381.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 97.2301(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.37210(10)
_cell_length_b                   13.30639(19)
_cell_length_c                   17.1682(2)
_cell_measurement_reflns_used    4168
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.7190
_cell_measurement_theta_min      4.1970
_cell_volume                     1670.74(4)
_computing_cell_refinement
'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) [1]'
_computing_data_collection
'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) [1]'
_computing_data_reduction
'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [3]'
_computing_structure_solution    'ShelXT-2015 [4]'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -77.00  38.00   1.00    1.00    --  -40.81  19.00  90.00  115
  2  \w     67.00  93.00   1.00    1.00    --   40.81-125.00-150.00   26
  3  \w     72.00 113.00   1.00    1.00    --   40.81 165.00-109.00   41
  4  \w      1.00  53.00   1.00    1.00    --   40.81 -99.00-150.00   52
  5  \w     35.00  74.00   1.00    1.00    --  107.77-125.00 -90.00   39
  6  \w     78.00 134.00   1.00    1.00    --  107.77 -45.00-180.00   56
  7  \w     99.00 124.00   1.00    1.00    --  107.77 125.00  30.00   25
  8  \w     36.00 104.00   1.00    1.00    --  107.77 -95.00-180.00   68
  9  \w     98.00 145.00   1.00    1.00    --  107.77 118.00-166.00   47
 10  \w     29.00  60.00   1.00    1.00    --  107.77 -95.00 150.00   31
 11  \w     55.00 112.00   1.00    1.00    --  107.77-125.00  90.00   57
 12  \w     37.00 136.00   1.00    1.00    --  107.77 -30.00 -90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046451000
_diffrn_orient_matrix_UB_12      0.0996887000
_diffrn_orient_matrix_UB_13      -0.0459566000
_diffrn_orient_matrix_UB_21      -0.0649531000
_diffrn_orient_matrix_UB_22      -0.0567255000
_diffrn_orient_matrix_UB_23      -0.0766561000
_diffrn_orient_matrix_UB_31      -0.2002401000
_diffrn_orient_matrix_UB_32      0.0160391000
_diffrn_orient_matrix_UB_33      0.0139573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6479
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.821
_diffrn_reflns_theta_min         4.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       cube
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0357
_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/[\s^2^(Fo^2^)+(0.0598P)^2^+0.4928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3022
_reflns_number_total             3313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0873_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105242
_chemical_oxdiff_formula         'C H N O Cl'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C5(H5A), C7(H7), C8(H8), C10(H10), C11(H11),
 C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5B)
;