The crystal structure of 3-(1-(2-(4-hydroxy-3,5-dimethoxybenzylidene)hydrazinyl)ethylidene)chroman-2,4-dione dihydrate, C20H22N2O8
Radnović, Nikola D.; Dekić, Biljana R.; Ristić, Milenko N.; Sejmanović, Dragana M.; Aksić, Marija S.; Krüger, Biljana; Rodić, Marko V.; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 171–173; doi:10.1515/ncrs-2022-0594

data_8107385
_publ_section_title
;
 The crystal structure of
 3-(1-(2-(4-hydroxy-3,5-dimethoxybenzylidene)hydrazinyl)ethylidene)chroman-2,4-dione
 dihydrate, C20H22N2O8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              171
_journal_page_last               173
_journal_paper_doi               10.1515/ncrs-2022-0594
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C20 H18 N2 O6, 2(H2 O)'
_chemical_formula_sum            'C20 H22 N2 O8'
_chemical_formula_weight         418.39
_chemical_name_common
;
3-(1-(2-(4-hydoxy-3,5-dimethoxybenzylidene)hydrazinyl)ethylidene)chroman-2,4-
dione dihydrate
;
_chemical_name_systematic
;
3-(1-(2-(4-hydoxy-3,5-dimethoxybenzylidene)hydrazinyl)ethylidene)chroman-2,4-
dione dihydrate
;
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   .
_audit_creation_method           'punched by SHELXL-2018/3 and manually edited'
_cell_angle_alpha                90
_cell_angle_beta                 100.013(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7634(8)
_cell_length_b                   17.9290(18)
_cell_length_c                   12.8437(9)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.3400
_cell_measurement_theta_min      3.2340
_cell_volume                     1987.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a [1]'
_computing_data_collection       'CrysAlisPro 1.171.41.93a [1]'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a [1]'
_computing_molecular_graphics    'PLATON [4]'
_computing_publication_material  'PLATON [4]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT 2018/2 [2]'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3575
_diffrn_detector_type            'Ruby (Oxford Diffraction)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -23.00  13.00   1.00   10.00    --    9.94  77.00  30.00   36
  2  \w     18.00  84.00   1.00   10.00    --    9.94  38.00-120.00   66
  3  \w    -19.00   7.00   1.00   10.00    --    9.94  77.00   0.00   26
  4  \w     -7.00  63.00   1.00   10.00    --    9.94  38.00-180.00   70
  5  \w    -85.00 -35.00   1.00   10.00    --  -11.66 179.00 120.00   50
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Gemini R ultra (Oxford Diffraction)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0509424000
_diffrn_orient_matrix_UB_12      -0.0308568000
_diffrn_orient_matrix_UB_13      -0.0105176000
_diffrn_orient_matrix_UB_21      0.0642586000
_diffrn_orient_matrix_UB_22      -0.0240414000
_diffrn_orient_matrix_UB_23      -0.0003047000
_diffrn_orient_matrix_UB_31      0.0051550000
_diffrn_orient_matrix_UB_32      -0.0060648000
_diffrn_orient_matrix_UB_33      0.0550665000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12227
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.619
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.41.93a [1] 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.680
_exptl_crystal_size_mid          0.459
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0140(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 [3]'
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0401
_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/[\s^2^(Fo^2^)+(0.0476P)^2^+0.4361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3154
_reflns_number_total             4053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0594_suppl.cif
_cod_data_source_block           V
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8107385
_shelxl_version_number           2018/3
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              73248
_shelx_hkl_checksum              82788