The crystal structure of [(2,2′-bipyridine-6-carboxylato-κ3 N,N,O)-(6-phenylpyridine-2-carboxylate-κ2 N,O)copper(II)] monohydrate, C23H17N3O5Cu
Zeng-Bing, Zhao; Xue-Ping, Li; Shu-Cheng, Yang; Bing-Qi, Yang; Ze-Tao, Wang; Lan-Xing, Cheng; Xi-Shi, Tai; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 615–617; doi:10.1515/ncrs-2023-0118

data_8107511
_publ_section_title
;
 The crystal structure of [(2,2&#x2032;-bipyridine-6-carboxylato-\k3
 N,N,O)-(6-phenylpyridine-2-carboxylate-\k2 N,O)copper(II)] monohydrate,
 C23H17N3O5Cu
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              615
_journal_page_last               617
_journal_paper_doi               10.1515/ncrs-2023-0118
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C23 H15 Cu N3 O4, H2 O'
_chemical_formula_sum            'C23 H17 Cu N3 O5'
_chemical_formula_weight         478.93
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.4330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.49510(10)
_cell_length_b                   8.69660(10)
_cell_length_c                   21.1454(2)
_cell_measurement_reflns_used    12409
_cell_measurement_temperature    294.10(10)
_cell_measurement_theta_max      75.5200
_cell_measurement_theta_min      3.9820
_cell_volume                     2037.65(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.10(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.953
_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    100.00 171.00   0.50    1.00    --  109.26  61.00 120.00  142
  2  \w     82.00 120.00   0.50    1.00    --  109.26 149.00 150.00   76
  3  \w    113.00 145.00   0.50    1.00    --  109.26 123.00 -12.00   64
  4  \w     98.00 131.00   0.50    1.00    --  109.26 125.00 -90.00   66
  5  \w    -30.00  26.00   0.50    0.32    --   43.18 -19.00 120.00  112
  6  \w     35.00  60.00   0.50    1.00    --  109.26 -61.00  30.00   50
  7  \w     35.00 106.00   0.50    1.00    --  109.26 -77.00  60.00  142
  8  \w     35.00  70.00   0.50    1.00    --  109.26 -61.00  60.00   70
  9  \w     38.00  70.00   0.50    1.00    --  109.26 -61.00 -30.00   64
 10  \w     40.00  66.00   0.50    1.00    --  109.26 -61.00 -60.00   52
 11  \w     43.00  71.00   0.50    1.00    --  109.26 -61.00 -90.00   56
 12  \w     35.00  92.00   0.50    1.00    --  109.26 -77.00-120.00  114
 13  \w    -21.00  42.00   0.50    0.32    --   43.18 -37.00-150.00  126
 14  \w     41.00  66.00   0.50    0.32    --   43.18-123.00 -93.00   50
 15  \w     39.00 107.00   0.50    1.00    --  109.26-125.00-120.00  136
 16  \w     72.00 101.00   0.50    1.00    --  109.26-123.00 -93.00   58
 17  \w     64.00  89.00   0.50    1.00    --  109.26-149.00 103.00   50
 18  \w     55.00  80.00   0.50    0.32    --   43.18-149.00 103.00   50
 19  \w    -51.00 -16.00   0.50    1.00    --  -90.25  45.00 150.00   70
 20  \w    -49.00 -15.00   0.50    1.00    --  -90.25  45.00 120.00   68
 21  \w   -102.00 -25.00   0.50    0.32    --  -43.18 149.00 150.00  154
 22  \w    -61.00 -35.00   0.50    0.32    --  -43.18 123.00 -12.00   52
 23  \w    -51.00 -14.00   0.50    1.00    --  -90.25  45.00  30.00   74
 24  \w    -80.00 -55.00   0.50    0.32    --  -43.18 -57.00 -60.00   50
 25  \w   -116.00 -14.00   0.50    0.32    --  -43.18 -77.00  90.00  204
 26  \w   -111.00 -86.00   0.50    0.32    --  -43.18 -57.00 -60.00   50
 27  \w   -113.00 -86.00   0.50    1.00    --  -90.25 -61.00-180.00   54
 28  \w   -143.00-117.00   0.50    1.00    --  -90.25 -61.00-180.00   52
 29  \w   -133.00 -75.00   0.50    1.00    --  -90.25-123.00 -93.00  116
 30  \w   -122.00 -96.00   0.50    1.00    --  -90.25-149.00 103.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0818385000
_diffrn_orient_matrix_UB_12      0.0342862000
_diffrn_orient_matrix_UB_13      0.0453315000
_diffrn_orient_matrix_UB_21      -0.1030657000
_diffrn_orient_matrix_UB_22      0.0455590000
_diffrn_orient_matrix_UB_23      -0.0600529000
_diffrn_orient_matrix_UB_31      -0.0448116000
_diffrn_orient_matrix_UB_32      -0.1677490000
_diffrn_orient_matrix_UB_33      -0.0070433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14284
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.722
_diffrn_reflns_theta_min         4.002
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0039(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.7197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3836
_reflns_number_total             4042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0118_suppl_001.cif
_cod_data_source_block           1-1
_cod_database_code               8107511
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 H1A-H1B
 1.34 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C15(H15),
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              66627
_shelx_hkl_checksum              92864
_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 1.800
_oxdiff_exptl_absorpt_empirical_full_min 0.647