Crystal structure of the Cu(II) complex chlorido-(6-oxo-2-phenyl-1,6-dihydropyrimidine-4-carboxylato-k2 N,O)-(phenanthroline-k2 N,N')copper(II), C23H15ClCuN4O3
Yang, Qi; Hou, Meng-Qi; Chen, Pei-Rou; Li, Shuo; Zhou, Guang-Peng; Li, Gan; Chen, Dong-Dong; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 109–111; doi:10.1515/ncrs-2020-0398

data_8104896
_publ_section_title
;
 Crystal structure of the Cu(II) complex
 chlorido-(6-oxo-2-phenyl-1,6-dihydropyrimidine-4-carboxylato-k2
 N,O)-(phenanthroline-k2 N,N')copper(II), C23H15ClCuN4O3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              109
_journal_page_last               111
_journal_paper_doi               10.1515/ncrs-2020-0398
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C23 H15 Cl Cu N4 O3'
_chemical_formula_sum            'C23 H15 Cl Cu N4 O3'
_chemical_formula_weight         494.38
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 116.2165(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.63346(14)
_cell_length_b                   17.99387(15)
_cell_length_c                   11.60320(16)
_cell_measurement_reflns_used    9400
_cell_measurement_temperature    292.88(11)
_cell_measurement_theta_max      71.8140
_cell_measurement_theta_min      4.6220
_cell_volume                     1991.74(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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_environment      air
_diffrn_ambient_temperature      292.88(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -103.00 -19.00   1.00    1.09    --  -35.97 -57.00 -90.00   84
  2  \w      1.00  75.00   1.00    1.09    --   35.97 -99.00 150.00   74
  3  \w    -32.00  63.00   1.00    1.09    --   35.97 -77.00   0.00   95
  4  \w     24.00  90.00   1.00    1.09    --   35.97-126.00 -30.00   66
  5  \w     17.00 105.00   1.00    1.09    --   35.97  38.00  90.00   88
  6  \w     91.00 176.00   1.00    4.38    --  107.97  45.00 120.00   85
  7  \w     40.00 135.00   1.00    4.38    --  107.97 -77.00  90.00   95
  8  \w     57.00 150.00   1.00    4.38    --  107.97 178.00 150.00   93
  9  \w     39.00 110.00   1.00    4.38    --  107.97 -95.00-120.00   71
 10  \w     90.00 175.00   1.00    4.38    --  107.97  61.00 -30.00   85
 11  \w     90.00 175.00   1.00    4.38    --  107.97  61.00-120.00   85
 12  \w     90.00 175.00   1.00    4.38    --  107.97  61.00   0.00   85
 13  \w     39.00 110.00   1.00    4.38    --  107.97 -95.00 150.00   71
 14  \w   -104.00  -9.00   1.00    1.09    --  -35.97 -77.00   0.00   95
 15  \w   -103.00 -19.00   1.00    1.09    --  -35.97 -57.00-150.00   84
 16  \w   -104.00  -9.00   1.00    1.09    --  -35.97 -77.00 150.00   95
 17  \w    -31.00  53.00   1.00    1.09    --   35.97 -57.00-150.00   84
 18  \w     91.00 176.00   1.00    4.38    --  107.97  45.00-180.00   85
 19  \w     91.00 172.00   1.00    4.38    --  107.97  45.00 -60.00   81
 20  \w     90.00 175.00   1.00    4.38    --  107.97  61.00  60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0127590000
_diffrn_orient_matrix_UB_12      -0.0803155000
_diffrn_orient_matrix_UB_13      -0.0499247000
_diffrn_orient_matrix_UB_21      0.1414411000
_diffrn_orient_matrix_UB_22      0.0082268000
_diffrn_orient_matrix_UB_23      -0.0055165000
_diffrn_orient_matrix_UB_31      0.0769003000
_diffrn_orient_matrix_UB_32      -0.0285095000
_diffrn_orient_matrix_UB_33      0.1392038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.712
_diffrn_reflns_theta_min         4.635
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.9430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3568
_reflns_number_total             3863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0398_suppl.cif
_cod_data_source_block           1
_cod_database_code               8104896
_chemical_oxdiff_formula         'C1 H1 N1 Cu1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C23(H23), C2(H2), C3(H3), C19(H19), C6(H6), C22(H22),
 C10(H10), C8(H8), C9(H9), C5(H5), C20(H20), C21(H21)
;
_shelx_shelxl_version_number     2017/1