The crystal structure of bis(benzoato-κ2 O,O′)-(2,9-dimethyl-1,10-phenanthroline-κ2 N,N′)-copper(II), C28H22CuN2O4
Yang, Fei; Liu, Pengju; Guo, Libing; Xian, Dong; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1219–1221; doi:10.1515/ncrs-2021-0283

data_8104570
_publ_section_title
;
 The crystal structure of bis(benzoato-\k2
 O,O&#x2032;)-(2,9-dimethyl-1,10-phenanthroline-\k2
 N,N&#x2032;)-copper(II), C28H22CuN2O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1219
_journal_page_last               1221
_journal_paper_doi               10.1515/ncrs-2021-0283
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C14 H11 Cu0.5 N O2'
_chemical_formula_sum            'C14 H11 Cu0.5 N O2'
_chemical_formula_weight         257.01
_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                 90.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2971(3)
_cell_length_b                   14.4409(3)
_cell_length_c                   9.5617(2)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.3380
_cell_measurement_theta_min      6.0750
_cell_volume                     2388.25(8)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009) [1]'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009) [1]'
_computing_molecular_graphics    'Diamond 3.2i [2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [3]'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018) [4]'
_computing_structure_solution    'SHELXS  (Sheldrick, 2018) [5]'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_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    -76.00  18.00   1.00    1.00    --  -35.62 101.00  55.00   94
  2  \w      4.00  76.00   1.00    1.00    --   35.62-101.00 -48.00   72
  3  \w     37.00 110.00   1.00    3.26    --  107.12-101.00 -48.00   73
  4  \w    101.00 177.00   1.00    3.26    --  107.12 101.00  55.00   76
  5  \w   -105.00 -17.00   1.00    1.00    --  -35.62 -38.00-150.00   88
  6  \w   -107.00 -36.00   1.00    1.00    --  -35.62-178.00 120.00   71
  7  \w     59.00 107.00   1.00    1.00    --   35.62-178.00-120.00   48
  8  \w     59.00  85.00   1.00    3.26    --  107.12 -95.00-120.00   26
  9  \w     97.00 173.00   1.00    3.26    --  107.12  61.00  90.00   76
 10  \w    149.00 176.00   1.00    3.26    --  107.12 111.00 -30.00   27
 11  \w    102.00 131.00   1.00    3.26    --  107.12 111.00 -30.00   29
 12  \w     42.00  82.00   1.00    3.26    --  107.12 -95.00  60.00   40
 13  \w     43.00 101.00   1.00    3.26    --  107.12 -61.00 -60.00   58
 14  \w     81.00 175.00   1.00    3.26    --  107.12  77.00-150.00   94
 15  \w     43.00 123.00   1.00    3.26    --  107.12 -61.00  90.00   80
;
_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      0.0253489000
_diffrn_orient_matrix_UB_12      -0.1016017000
_diffrn_orient_matrix_UB_13      -0.0177142000
_diffrn_orient_matrix_UB_21      -0.0476144000
_diffrn_orient_matrix_UB_22      -0.0063542000
_diffrn_orient_matrix_UB_23      -0.1367664000
_diffrn_orient_matrix_UB_31      0.0708494000
_diffrn_orient_matrix_UB_32      0.0320180000
_diffrn_orient_matrix_UB_33      -0.0833044000
_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  0.0172
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5189
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.428
_diffrn_reflns_theta_min         3.988
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.213
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0736P)^2^+2.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2084
_reflns_number_total             2261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0283_suppl.cif
_cod_data_source_block           rmm-20210702
_cod_original_formula_sum        'C14 H11 Cu0.50 N O2'
_cod_database_code               8104570
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              48115
_shelx_hkl_checksum              1107
_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.802