The crystal structure of aqua-bis(3-acetyl-2-oxo-2H-chromen-4-olato-κ2 O,O′)zinc(II) monohydrate, C22H18O10Zn
Ristić, Milenko N.; Rodić, Marko V.; Radulović, Niko S.; Dekić, Biljana R.; Dekić, Vidoslav S.; Ristić, Novica R.; Gurešić, Dejan M.; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 729–731; doi:10.1515/ncrs-2019-0077

data_8105833
_publ_section_title
;
 The crystal structure of aqua-bis(3-acetyl-2-oxo-2H-chromen-4-olato-\k2
 O,O&#x2032;)zinc(II) monohydrate, C22H18O10Zn
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              729
_journal_page_last               731
_journal_paper_doi               10.1515/ncrs-2019-0077
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C22 H16 O9 Zn, H2 O'
_chemical_formula_sum            'C22 H18 O10 Zn'
_chemical_formula_weight         507.73
_chemical_name_common
' aquabis(3-acetyl-4-hydroxycoumarino)zinc(II) monohydrate'
_chemical_name_systematic
' aquabis(3-acetyl-2-oxo-2H-chromen-4-olate)zinc(II) monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   .
_cell_angle_alpha                81.713(3)
_cell_angle_beta                 82.724(3)
_cell_angle_gamma                73.103(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9616(3)
_cell_length_b                   9.5386(3)
_cell_length_c                   14.2569(4)
_cell_measurement_reflns_used    10583
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.3010
_cell_measurement_theta_min      2.7970
_cell_volume                     1021.03(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 [1]'
_computing_data_collection       'CrysAlisPro 1.171.39.46 [1]'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 [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      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3280
_diffrn_detector_type            'Sapphire3 (Oxford Diffraction)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -25.00  23.00   0.80   15.00    --  -16.43 -99.00  90.00   60
  2  \w    -25.00  23.00   0.80   15.00    --  -16.43 -99.00   0.00   60
  3  \w    -10.00  84.40   0.80   15.00    --   17.14  77.00 -30.00  118
  4  \w    -50.00  34.00   0.80   15.00    --   17.14 -57.00  90.00  105
  5  \w    -25.00  55.00   0.80   15.00    --   17.14 -99.00  60.00  100
  6  \w    -50.00  43.60   0.80   15.00    --   17.14 -77.00-150.00  117
  7  \w    -33.00  51.00   0.80   15.00    --  -16.43  57.00 -60.00  105
  8  \w      0.00  84.00   0.80   15.00    --   17.14  57.00 120.00  105
  9  \w      0.00  84.00   0.80   15.00    --   17.14  57.00-120.00  105
 10  \w    -25.00  55.00   0.80   15.00    --   17.14 -99.00-150.00  100
 11  \w      0.00  84.00   0.80   15.00    --   17.14  57.00-150.00  105
 12  \w    -25.00  36.60   0.80   15.00    --   17.14 -99.00 120.00   77
 13  \w    -25.00  55.00   0.80   15.00    --   17.14 -99.00 -30.00  100
 14  \f    -30.00 239.60   0.80    0.40   0.00   0.00   0.00    --   337
;
_diffrn_measurement_device_type  'Gemini S (Oxford Diffraction)'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0037025000
_diffrn_orient_matrix_UB_12      0.0527560000
_diffrn_orient_matrix_UB_13      -0.0401526000
_diffrn_orient_matrix_UB_21      -0.0769716000
_diffrn_orient_matrix_UB_22      -0.0101853000
_diffrn_orient_matrix_UB_23      -0.0148389000
_diffrn_orient_matrix_UB_31      -0.0529263000
_diffrn_orient_matrix_UB_32      0.0568428000
_diffrn_orient_matrix_UB_33      0.0267522000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.315
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.532
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type
'Enhance (Mo) X-ray Source (Oxford Diffraction)'
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
 Analytical numeric absorption correction using a multifaceted crystal 
 model based on expressions derived by R.C. Clark & J.S. Reid. 
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897), followed
 by empirical absorption correction using spherical harmonics
 (Blessing, B. (1995) Acta Cryst. A51, 33--38), 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4157
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.3621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3901
_reflns_number_total             4157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0077_suppl.cif
_cod_data_source_block           VD-D_2202_p_abs
_cod_database_code               8105833
_shelx_estimated_absorpt_t_min   0.595
_shelx_estimated_absorpt_t_max   0.893
_oxdiff_exptl_absorpt_empirical_full_min 0.962
_oxdiff_exptl_absorpt_empirical_full_max 1.035
_oxdiff_exptl_absorpt_empirical_details
; Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              77704
_shelx_hkl_checksum              73785