The crystal structure of bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-κ 2 N,O)-copper(ii), C14H8N6O4Cu
Hong, Dong-Feng; Chen, Ye; Zhu, Wen-Li; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 679–680; doi:10.1515/ncrs-2022-0178

data_8107186
_publ_section_title
;
 The crystal structure of bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-\k 2
 N,O)-copper(ii), C14H8N6O4Cu
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              679
_journal_page_last               680
_journal_paper_doi               10.1515/ncrs-2022-0178
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C14 H8 Cu N6 O4'
_chemical_formula_sum            'C14 H8 Cu N6 O4'
_chemical_formula_weight         387.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 108.550(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6054(8)
_cell_length_b                   7.0441(3)
_cell_length_c                   12.6301(6)
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9440
_cell_measurement_theta_min      4.3270
_cell_volume                     1316.25(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.904
_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    -83.00   3.00   1.00    2.00    --  -15.84 -38.00 120.00   86
  2  \w    -35.00  53.00   1.00    2.00    --  -15.84  38.00 -60.00   88
  3  \w    -69.00  -6.00   1.00    2.00    --  -15.84 124.00 166.25   63
  4  \w    -11.00  82.00   1.00    2.00    --   17.09  19.00 -30.00   93
  5  \w     18.00  86.00   1.00    2.00    --   17.09  38.00  60.00   68
  6  \w     -8.00  37.00   1.00    2.00    --   17.09  77.00 -90.00   45
  7  \w     -6.00  56.00   1.00    2.00    --   17.09 -99.00 150.00   62
  8  \w    -10.00  15.00   1.00    2.00    --   17.09  77.00 120.00   25
;
_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      -0.0149193000
_diffrn_orient_matrix_UB_12      -0.0921498000
_diffrn_orient_matrix_UB_13      0.0084780000
_diffrn_orient_matrix_UB_21      0.0392781000
_diffrn_orient_matrix_UB_22      -0.0397627000
_diffrn_orient_matrix_UB_23      -0.0079514000
_diffrn_orient_matrix_UB_31      0.0231194000
_diffrn_orient_matrix_UB_32      0.0080308000
_diffrn_orient_matrix_UB_33      0.0580763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7521
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.361
_diffrn_reflns_theta_min         3.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    1.957
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0304P)^2^+2.0704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1460
_reflns_number_total             1631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0178_suppl.cif
_cod_data_source_block           hdf20
_cod_original_cell_volume        1316.24(11)
_cod_database_code               8107186
_shelx_estimated_absorpt_t_max   0.630
_shelx_estimated_absorpt_t_min   0.588
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7)
;
_shelx_res_checksum              2695
_shelx_hkl_checksum              83755
_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.776