The crystal structure of poly[diaqua-(μ3-5-nitrobenzene-1,2,3-tricarboxylato-κ 3 O:O′:O′)-(μ2-4,4′-dipyridylamine-κ 2 N:N′)copper(II)], C38H30Cu3N8O20
Hong, Dong-Feng; Chen, Ye; Zhu, Wen-Li; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 429–431; doi:10.1515/ncrs-2022-0040

data_8105715
_publ_section_title
;
 The crystal structure of
 poly[diaqua-(\m3-5-nitrobenzene-1,2,3-tricarboxylato-\k 3
 O:O&#x2032;:O&#x2032;)-(\m2-4,4&#x2032;-dipyridylamine-\k 2
 N:N&#x2032;)copper(II)], C38H30Cu3N8O20
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              429
_journal_page_last               431
_journal_paper_doi               10.1515/ncrs-2022-0040
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C38 H30 Cu3 N8 O20'
_chemical_formula_sum            'C38 H30 Cu3 N8 O20'
_chemical_formula_weight         1109.32
_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
_cell_angle_alpha                77.466(3)
_cell_angle_beta                 73.915(3)
_cell_angle_gamma                75.794(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2659(3)
_cell_length_b                   11.7245(3)
_cell_length_c                   12.6837(4)
_cell_measurement_reflns_used    6478
_cell_measurement_temperature    290.7(3)
_cell_measurement_theta_max      27.7740
_cell_measurement_theta_min      3.7570
_cell_volume                     993.50(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      290.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_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    -11.00  16.00   1.00    8.00    --  -13.80 -99.00  30.00   27
  2  \w      0.00  82.00   1.00    8.00    --   14.82  57.00-120.00   82
  3  \w    -52.00  -1.00   1.00    8.00    --   14.82 -77.00-120.00   51
  4  \w     -1.00  78.00   1.00    8.00    --   14.82  57.00 -30.00   79
  5  \w    -20.00  54.00   1.00    8.00    --   14.82 -99.00 150.00   74
  6  \w     21.00  81.00   1.00    8.00    --   14.82  57.00  30.00   60
  7  \w    -14.00  54.00   1.00    8.00    --   14.82 -99.00  60.00   68
  8  \w    -12.00  54.00   1.00    8.00    --   14.82 -99.00 -90.00   66
  9  \w    -50.00  31.00   1.00    8.00    --   14.82 -57.00 -30.00   81
 10  \w      1.00  69.00   1.00    8.00    --   14.82  57.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0916696000
_diffrn_orient_matrix_UB_12      0.0120567000
_diffrn_orient_matrix_UB_13      -0.0012811000
_diffrn_orient_matrix_UB_21      -0.0257782000
_diffrn_orient_matrix_UB_22      0.0579840000
_diffrn_orient_matrix_UB_23      -0.0294891000
_diffrn_orient_matrix_UB_31      -0.0409072000
_diffrn_orient_matrix_UB_32      0.0221201000
_diffrn_orient_matrix_UB_33      0.0510394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12847
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       block
_exptl_crystal_F_000             561
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0383P)^2^+0.8939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3279
_reflns_number_total             3694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0040_suppl.cif
_cod_data_source_block           8101zi
_cod_database_code               8105715
_chemical_oxdiff_usercomment     Y202-Co
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 O(H,H) groups
2.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              25346
_shelx_hkl_checksum              33984
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.658