Crystal structure of bis(6-aminopyridine-2-carboxylato-κ2 O,N)-copper(II), C12H10O6N4Cu
Du, Xigang; Wang, Chunwei; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1007–1008; doi:10.1515/ncrs-2020-0041

data_8105361
_publ_section_title
;
 Crystal structure of bis(6-aminopyridine-2-carboxylato-\k2
 O,N)-copper(II), C12H10O6N4Cu
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1007
_journal_page_last               1008
_journal_paper_doi               10.1515/ncrs-2020-0041
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 Cu N4 O4'
_chemical_formula_sum            'C12 H10 Cu N4 O4'
_chemical_formula_weight         337.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.060(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7015(2)
_cell_length_b                   7.3920(4)
_cell_length_c                   21.3535(12)
_cell_measurement_reflns_used    2417
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.7200
_cell_measurement_theta_min      3.9560
_cell_volume                     584.16(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      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -81.00   2.00   1.00   16.56    --  -13.80 -57.00  60.00   83
  2  \w     -2.00  24.00   1.00   16.56    --  -13.80 -99.00 120.00   26
  3  \w    -41.00  31.00   1.00   16.56    --  -13.80  77.00 -60.00   72
  4  \w    -81.00 -31.00   1.00   16.56    --  -13.80 -57.00   0.00   50
  5  \w    -81.00  14.00   1.00   16.56    --  -13.80 -19.00 120.00   95
  6  \w     -5.00  54.00   1.00   16.56    --   14.82 -99.00  60.00   59
;
_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      -0.1808896000
_diffrn_orient_matrix_UB_12      -0.0112102000
_diffrn_orient_matrix_UB_13      0.0096243000
_diffrn_orient_matrix_UB_21      0.0464142000
_diffrn_orient_matrix_UB_22      0.0375922000
_diffrn_orient_matrix_UB_23      0.0296519000
_diffrn_orient_matrix_UB_31      -0.0429152000
_diffrn_orient_matrix_UB_32      0.0875758000
_diffrn_orient_matrix_UB_33      -0.0115038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            4327
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47013
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0290P)^2^+0.7540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1016
_reflns_number_total             1086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0041_suppl.cif
_cod_data_source_block           20195198
_cod_database_code               8105361
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.600
_reflns_odcompleteness_completeness 99.06
_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,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;