Crystal structure of diaqua-bis(2,4-dinitrophenolato-κ2 O,O′)copper(II) 1.5 hydrate, C12H13CuN4O13.5
Liu, Xiao-Jing; Li, Wen-Yu; Guo, Zi-Yu; Liu, E.; Jian, Fang-Fang; Liang, Tongling; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 851–853; doi:10.1515/ncrs-2021-0093

data_8104732
_publ_section_title
;
 Crystal structure of diaqua-bis(2,4-dinitrophenolato-\k2
 O,O&#x2032;)copper(II) 1.5 hydrate, C12H13CuN4O13.5
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              851
_journal_page_last               853
_journal_paper_doi               10.1515/ncrs-2021-0093
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '2(C12 H10 Cu N4 O12), 3(H2 O)'
_chemical_formula_sum            'C24 H26 Cu2 N8 O27'
_chemical_formula_weight         985.603
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_cell_angle_alpha                61.225(3)
_cell_angle_beta                 85.342(2)
_cell_angle_gamma                83.938(2)
_cell_formula_units_Z            1
_cell_length_a                   4.7705(1)
_cell_length_b                   14.6219(5)
_cell_length_c                   14.7418(3)
_cell_measurement_reflns_used    5733
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      73.3750
_cell_measurement_theta_min      3.4450
_cell_volume                     895.73(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9625
_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   -120.00 -34.00   0.50    0.05    --  -46.95 -37.00-149.00  172
  2  \w    -31.00  -6.00   0.50    0.05    --  -46.95  37.00   6.00   50
  3  \w    -17.00  44.00   0.50    0.05    --   46.95 -37.00-149.00  122
  4  \w     37.00 120.00   0.50    0.05    --   46.95  37.00   6.00  166
  5  \w   -161.00-118.00   0.50    0.05    --  -99.00 -37.00-149.00   86
  6  \w    100.00 169.00   0.50    0.05    --  103.25  37.00   6.00  138
  7  \w    -52.00 -25.00   0.50    0.05    --  -46.95 125.00-180.00   54
  8  \w    -80.00 -55.00   0.50    0.05    --  -46.95 125.00-180.00   50
  9  \w    -19.00  27.00   0.50    0.05    --  -46.95  19.00 150.00   92
 10  \w    -24.00  61.00   0.50    0.05    --   46.95 -57.00  90.00  170
 11  \w    -72.00 -45.00   0.50    0.05    --  -99.00 125.00-150.00   54
 12  \w   -112.00 -67.00   0.50    0.05    --  -99.00 125.00  30.00   90
 13  \w    -85.00 -59.00   0.50    0.05    --  -99.00 125.00 -30.00   52
 14  \w   -102.00 -45.00   0.50    0.05    --  -99.00  77.00 -90.00  114
 15  \w   -110.00 -79.00   0.50    0.05    --  -99.00 125.00-150.00   62
 16  \w   -121.00 -45.00   0.50    0.05    --  -99.00 139.00-141.86  152
 17  \w   -112.00 -86.00   0.50    0.05    --  -99.00 125.00 -30.00   52
 18  \w   -112.00 -80.00   0.50    0.05    --  -99.00 125.00  90.00   64
 19  \w     31.00  78.00   0.50    0.05    --  103.25-125.00-150.00   94
 20  \w     32.00  69.00   0.50    0.05    --  103.25 -61.00   0.00   74
 21  \w     69.00  95.00   0.50    0.05    --  103.25 -94.00 -90.00   52
 22  \w     90.00 159.00   0.50    0.05    --  103.25  61.00-150.00  138
 23  \w     96.00 168.00   0.50    0.05    --  103.25  15.00 120.00  144
 24  \w     89.00 115.00   0.50    0.05    --  103.25 125.00-150.00   52
 25  \w    127.00 160.00   0.50    0.05    --  103.25  61.00 -60.00   66
 26  \w     32.00  92.00   0.50    0.05    --  103.25 -94.00   0.00  120
 27  \w     94.00 123.00   0.50    0.05    --  103.25  61.00 -60.00   58
 28  \w     33.00 100.00   0.50    0.05    --  103.25 -94.00 150.00  134
 29  \w     80.00 146.00   0.50    0.05    --  103.25 125.00  90.00  132
 30  \w     32.00 106.00   0.50    0.05    --  103.25 -94.00 -60.00  148
 31  \w     70.00  98.00   0.50    0.05    --  103.25 -94.00 120.00   56
 32  \w    123.00 150.00   0.50    0.05    --  103.25  45.00-150.00   54
 33  \w     91.00 118.00   0.50    0.05    --  103.25  45.00-150.00   54
 34  \w     34.00  68.00   0.50    0.05    --  103.25 -94.00 120.00   68
 35  \w    135.00 163.00   0.50    0.05    --  103.25 125.00-150.00   56
 36  \w     31.00  70.00   0.50    0.05    --  103.25-125.00 -30.00   78
 37  \w     31.00  75.00   0.50    0.05    --  103.25 -61.00  30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9625
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10333
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9625
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.38
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_description       plate
_exptl_crystal_F_000             498.106
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.0536
_refine_diff_density_min         -0.9086
_refine_diff_density_rms         0.1054
_refine_ls_d_res_high            0.7967
_refine_ls_d_res_low             12.9136
_refine_ls_goodness_of_fit_ref   1.0546
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0546
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.0021
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+0.8420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              18
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3306
_reflns_number_total             3542
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_j_ncrs-2021-0093_suppl.cif
_cod_data_source_block           TX4062A
_cod_database_code               8104732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O14(0.5) H14a(0.5) H14b(0.5)
3.a Riding coordinates:
 O14(H14a,H14b)
3.b Free rotating group:
 O13(H13a,H13b)
3.c Rotating group:
 O11(H11a,H11b), O12(H12a,H12b)
3.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;