Synthesis, structure and magnetic properties of two bis(oxalato)cuprate(ii) salts with pyridinium type counter ions
Dazem, Cyrielle L. F.; Inge, A. Ken; Luneau, Dominique; Öhrström, Lars; Nenwa, Justin; CrystEngComm 25 (2023) 1479–1485; doi:10.1039/D2CE01513G

data_7246012
_publ_section_title
;
 Synthesis, structure and magnetic properties of two
 bis(oxalato)cuprate(ii) salts with pyridinium type counter ions
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1479
_journal_page_last               1485
_journal_paper_doi               10.1039/D2CE01513G
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C2 Cu0.5 O4, C5 H7 N2 O'
_chemical_formula_sum            'C7 H7 Cu0.5 N2 O5'
_chemical_formula_weight         230.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-18
_audit_creation_method
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_audit_update_record
;
2022-11-04 deposited with the CCDC.	2022-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                86.127(3)
_cell_angle_beta                 77.266(4)
_cell_angle_gamma                81.424(4)
_cell_formula_units_Z            2
_cell_length_a                   5.0894(3)
_cell_length_b                   7.1344(3)
_cell_length_c                   11.4050(4)
_cell_measurement_reflns_used    4373
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.2020
_cell_measurement_theta_min      3.9190
_cell_volume                     399.15(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.954
_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    -29.00  32.00   0.50    0.42    --  -42.95  48.00 159.00  122
  2  \w   -118.00 -29.00   0.50    0.42    --  -42.95 -48.00  11.00  178
  3  \w   -174.00 -90.00   0.50    1.66    -- -104.50 -48.00  11.00  168
  4  \w     95.00 178.00   0.50    1.66    --  109.23  48.00 159.00  166
  5  \w    -15.00  34.00   0.50    0.42    --  -42.95  38.00 -60.00   98
  6  \w    -15.00  34.00   0.50    0.42    --  -42.95  38.00 120.00   98
  7  \w    -32.00  36.00   0.50    0.42    --   42.95 -48.00  11.00  136
  8  \w     29.00  60.00   0.50    0.42    --   42.95  55.00-114.47   62
  9  \w     28.00  60.00   0.50    0.42    --   42.95  59.00 -76.11   64
 10  \w     30.00 118.00   0.50    0.42    --   42.95  48.00 159.00  176
 11  \w      3.00  77.00   0.50    0.42    --   42.95 -99.00-120.00  148
 12  \w      3.00  77.00   0.50    0.42    --   42.95 -99.00  60.00  148
 13  \w   -102.00 -31.00   0.50    1.66    -- -104.50 125.00-180.00  142
 14  \w   -132.00 -89.00   0.50    1.66    -- -104.50 -15.00 -60.00   86
 15  \w    -72.00 -30.00   0.50    1.66    -- -104.50  77.00 -30.00   84
 16  \w   -102.00 -31.00   0.50    1.66    -- -104.50 125.00   0.00  142
 17  \w   -132.00 -89.00   0.50    1.66    -- -104.50 -15.00-150.00   86
 18  \w   -132.00 -89.00   0.50    1.66    -- -104.50 -15.00 -90.00   86
 19  \w    -72.00 -30.00   0.50    1.66    -- -104.50  77.00   0.00   84
 20  \w    -72.00 -30.00   0.50    1.66    -- -104.50  77.00 120.00   84
 21  \w   -174.00 -91.00   0.50    1.66    -- -104.50-125.00-180.00  166
 22  \w    -72.00 -30.00   0.50    1.66    -- -104.50  77.00 150.00   84
 23  \w   -132.00 -89.00   0.50    1.66    -- -104.50 -15.00-120.00   86
 24  \w   -102.00 -31.00   0.50    1.66    -- -104.50 125.00-150.00  142
 25  \w    -72.00 -30.00   0.50    1.66    -- -104.50  77.00-150.00   84
 26  \w   -102.00 -31.00   0.50    1.66    -- -104.50 125.00  90.00  142
 27  \w   -102.00 -31.00   0.50    1.66    -- -104.50 125.00  30.00  142
 28  \w     35.00  93.00   0.50    1.66    --  109.23 -95.00   0.00  116
 29  \w     35.00  93.00   0.50    1.66    --  109.23 -95.00 -60.00  116
 30  \w     95.00 170.00   0.50    1.66    --  109.23  30.00-150.00  150
 31  \w     35.00  93.00   0.50    1.66    --  109.23 -95.00-180.00  116
 32  \w     35.00  95.00   0.50    1.66    --  109.23 -91.00 120.20  120
 33  \w    -15.00  34.00   0.50    0.42    --  -42.95  38.00   0.00   98
 34  \w    -15.00  34.00   0.50    0.42    --  -42.95  38.00-150.00   98
 35  \w     29.00  60.00   0.50    0.42    --   42.95  55.00  42.38   62
 36  \w     27.00  54.00   0.50    0.42    --   42.95  61.00-174.83   54
 37  \w     30.00 118.00   0.50    0.42    --   42.95  48.00 -81.27  176
 38  \w     30.00 117.00   0.50    0.42    --   42.95  50.00 -30.26  174
 39  \w     29.00  60.00   0.50    0.42    --   42.95  56.00   5.49   62
 40  \w     28.00  60.00   0.50    0.42    --   42.95  59.00  91.21   64
 41  \w     28.00  60.00   0.50    0.42    --   42.95  57.00-134.23   64
 42  \w     30.00 120.00   0.50    0.42    --   42.95  38.00  90.00  180
 43  \w   -174.00 -90.00   0.50    1.66    -- -104.50 -45.00 -60.00  168
 44  \w   -174.00 -90.00   0.50    1.66    -- -104.50 -47.00-148.99  168
 45  \w   -174.00 -90.00   0.50    1.66    -- -104.50 -45.00-120.00  168
 46  \w   -173.00 -91.00   0.50    1.66    -- -104.50 -41.00  62.98  164
 47  \w   -174.00 -90.00   0.50    1.66    -- -104.50 -45.00 -90.00  168
 48  \w     95.00 170.00   0.50    1.66    --  109.23  30.00   0.00  150
 49  \w     94.00 139.00   0.50    1.66    --  109.23  15.00 150.00   90
 50  \w     94.00 139.00   0.50    1.66    --  109.23  15.00  60.00   90
 51  \w     94.00 139.00   0.50    1.66    --  109.23  15.00 120.00   90
 52  \w     94.00 139.00   0.50    1.66    --  109.23  15.00  90.00   90
 53  \w     95.00 178.00   0.50    1.66    --  109.23  45.00 150.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0944103000
_diffrn_orient_matrix_UB_12      -0.1935536000
_diffrn_orient_matrix_UB_13      -0.0069287000
_diffrn_orient_matrix_UB_21      0.2766171000
_diffrn_orient_matrix_UB_22      -0.0704070000
_diffrn_orient_matrix_UB_23      -0.0814904000
_diffrn_orient_matrix_UB_31      0.1128978000
_diffrn_orient_matrix_UB_32      -0.0730071000
_diffrn_orient_matrix_UB_33      0.1118660000
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6951
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.404
_diffrn_reflns_theta_min         3.976
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       needle
_exptl_crystal_F_000             235
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0612P)^2^+0.2309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1449
_reflns_number_total             1571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01513g2.cif
_cod_data_source_block           daz10_cu1_auto
_cod_depositor_comments
'Adding full bibliography for 7246009--7246013.cif.'
_cod_original_formula_sum        'C7 H7 Cu0.50 N2 O5'
_cod_database_code               7246012
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C16  H8  Cu1  N2  O10  '
_chemical_oxdiff_usercomment     'brown crystals'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11)
;
_shelx_res_checksum              37609
_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 1.790
_oxdiff_exptl_absorpt_empirical_full_min 0.651