Crystal structure of poly[(μ2-1-(1-imidazolyl)-4-(imidazol-1-ylmethyl)benzene-κ2 N:N′)-(μ3-pyridazine-4,5-dicarboxylate-κ3 O:O′:N)]copper(II) hydrate, C19H16CuN6O5
Liu, Guang-Zhen; Wang, Xiu-Jin; Wei, Wen-Hui; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 681–683; doi:10.1515/ncrs-2022-0106

data_8107187
_publ_section_title
;
 Crystal structure of
 poly[(\m2-1-(1-imidazolyl)-4-(imidazol-1-ylmethyl)benzene-\k2
 N:N&#x2032;)-(\m3-pyridazine-4,5-dicarboxylate-\k3
 O:O&#x2032;:N)]copper(II) hydrate, C19H16CuN6O5
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              681
_journal_page_last               683
_journal_paper_doi               10.1515/ncrs-2022-0106
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C19 H14 Cu N6 O4, H2 O'
_chemical_formula_sum            'C19 H16 Cu N6 O5'
_chemical_formula_weight         471.92
_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                82.900(3)
_cell_angle_beta                 74.593(3)
_cell_angle_gamma                83.612(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0143(3)
_cell_length_b                   9.2122(3)
_cell_length_c                   11.8205(4)
_cell_measurement_reflns_used    8778
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      3.9460
_cell_volume                     935.90(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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_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    -65.00 -34.00   1.00   15.00    --  -14.99 118.00 176.26   31
  2  \w    -40.00  52.00   1.00   15.00    --  -14.99  77.00  60.00   92
  3  \w    -70.00 -21.00   1.00   15.00    --  -14.99 127.00 -75.55   49
  4  \w    -33.00  56.00   1.00   15.00    --  -14.99  19.00 -90.00   89
  5  \w    -25.00  35.00   1.00   15.00    --  -14.99  57.00   0.00   60
  6  \w     13.00  84.00   1.00   15.00    --   16.08  38.00 150.00   71
  7  \w    -36.00  31.00   1.00   15.00    --   16.08 -57.00 150.00   67
  8  \w      6.00  81.00   1.00   15.00    --   16.08  57.00 -30.00   75
  9  \w     -6.00  83.00   1.00   15.00    --   16.08  77.00-150.00   89
 10  \w     -9.00  45.00   1.00   15.00    --   16.08  77.00  60.00   54
;
_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      -0.0183208000
_diffrn_orient_matrix_UB_12      -0.0101273000
_diffrn_orient_matrix_UB_13      0.0624852000
_diffrn_orient_matrix_UB_21      0.0427480000
_diffrn_orient_matrix_UB_22      -0.0695066000
_diffrn_orient_matrix_UB_23      -0.0025999000
_diffrn_orient_matrix_UB_31      0.0674049000
_diffrn_orient_matrix_UB_32      0.0335715000
_diffrn_orient_matrix_UB_33      -0.0007758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13542
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83944
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             482
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0247P)^2^+0.9246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3462
_reflns_number_total             3663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0106_suppl.cif
_cod_data_source_block           jfy-47
_cod_original_cell_volume        935.90(5)
_cod_database_code               8107187
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19)
;
_olex2_date_sample_data_collection 2018-10-29
_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 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.607