Crystal structure of bis(6-aminopyridine-2-carboxylato–k2O,N)-bis(N,N-dimethylformamide-k1 O)zinc(II), C18H24N6O6Zn
Hong, Dong-feng; Ye, Jia-Qi; Guo, Wen-Bo; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 529–531; doi:10.1515/ncrs-2023-0069

data_8107486
_publ_section_title
;
 Crystal structure of
 bis(6-aminopyridine-2-carboxylato--k2O,N)-bis(N,N-dimethylformamide-k1
 O)zinc(II), C18H24N6O6Zn
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              529
_journal_page_last               531
_journal_paper_doi               10.1515/ncrs-2023-0069
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C18 H24 N6 O6 Zn'
_chemical_formula_sum            'C18 H24 N6 O6 Zn'
_chemical_formula_weight         485.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.221(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1669(6)
_cell_length_b                   8.0831(4)
_cell_length_c                   13.1012(8)
_cell_measurement_reflns_used    3692
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.6610
_cell_measurement_theta_min      3.5820
_cell_volume                     1076.41(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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273(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 0.894
_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    -63.00 -25.00   1.00    7.00    --  -15.84 113.00 141.65   38
  2  \w    -23.00  53.00   1.00    7.00    --  -15.84  38.00 150.00   76
  3  \w    -83.00  -8.00   1.00    7.00    --  -15.84 -57.00 -30.00   75
  4  \w    -30.00  49.00   1.00    7.00    --  -15.84  57.00  60.00   79
  5  \w    -36.00   1.00   1.00    7.00    --  -15.84 -57.00   0.00   37
  6  \w    -23.00   5.00   1.00    7.00    --  -15.84 -77.00-120.00   28
  7  \w    -15.00  56.00   1.00    7.00    --   17.09 -99.00 -30.00   71
  8  \w    -43.00  30.00   1.00    7.00    --   17.09 -57.00-150.00   73
;
_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      0.0402538000
_diffrn_orient_matrix_UB_12      0.0218624000
_diffrn_orient_matrix_UB_13      0.0427932000
_diffrn_orient_matrix_UB_21      0.0337935000
_diffrn_orient_matrix_UB_22      0.0582014000
_diffrn_orient_matrix_UB_23      -0.0303088000
_diffrn_orient_matrix_UB_31      -0.0458989000
_diffrn_orient_matrix_UB_32      0.0619927000
_diffrn_orient_matrix_UB_33      0.0134109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10917
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.266
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67951
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0398P)^2^+0.1383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2018
_reflns_number_total             2615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0069_suppl_001.cif
_cod_data_source_block           2
_cod_database_code               8107486
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              29216
_shelx_hkl_checksum              61414
_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 3.534
_oxdiff_exptl_absorpt_empirical_full_min 0.340