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_7246013
_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         'C4 Cu O8, C13 H16 N2'
_chemical_formula_sum            'C17 H16 Cu N2 O8'
_chemical_formula_weight         439.86
_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
_audit_creation_date             2022-06-17
_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                90
_cell_angle_beta                 102.125(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5484(2)
_cell_length_b                   22.2344(6)
_cell_length_c                   7.22640(18)
_cell_measurement_reflns_used    10394
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      75.6290
_cell_measurement_theta_min      3.9850
_cell_volume                     1657.05(7)
_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      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_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     27.00  54.00   0.50    0.05    --   43.20  61.00 -51.26   54
  2  \w     28.00  56.00   0.50    0.05    --   43.20  60.00 -81.34   56
  3  \w     28.00  56.00   0.50    0.05    --   43.20  60.00-128.95   56
  4  \w     28.00  60.00   0.50    0.05    --   43.20  59.00-100.17   64
  5  \w     28.00  60.00   0.50    0.05    --   43.20  58.00 -26.72   64
  6  \w     28.00  60.00   0.50    0.05    --   43.20  59.00  -2.38   64
  7  \w     29.00  60.00   0.50    0.05    --   43.20  55.00-149.07   62
  8  \w     28.00  56.00   0.50    0.05    --   43.20  60.00  18.64   56
  9  \w     29.00  60.00   0.50    0.05    --   43.20  53.00  46.86   62
 10  \w     29.00  60.00   0.50    0.05    --   43.20  53.00  81.48   62
 11  \w     29.00  60.00   0.50    0.05    --   43.20  54.00 110.51   62
 12  \w     27.00  54.00   0.50    0.05    --   43.20  61.00 141.71   54
 13  \w     28.00  60.00   0.50    0.05    --   43.20  59.00 178.44   64
 14  \w     10.00  84.00   0.50    0.05    --   43.20-111.00 130.00  148
 15  \w     33.00  96.00   0.50    0.18    --  109.23-111.00 130.00  126
 16  \w     35.00  93.00   0.50    0.18    --  109.23 -95.00-180.00  116
 17  \w    -42.00  31.00   0.50    0.05    --  -43.20  57.00 120.00  146
 18  \w    -72.00 -30.00   0.50    0.18    -- -104.50  77.00 150.00   84
 19  \w    -72.00 -30.00   0.50    0.18    -- -104.50  77.00  60.00   84
 20  \w    -15.00  34.00   0.50    0.05    --  -43.20  38.00   0.00   98
 21  \w     94.00 139.00   0.50    0.18    --  109.23  15.00 -90.00   90
 22  \w    105.00 178.00   0.50    0.18    --  109.23 111.00-135.00  146
 23  \w     35.00  79.00   0.50    0.18    --  109.23 -77.00 -30.00   88
 24  \w     35.00  79.00   0.50    0.18    --  109.23 -77.00 -60.00   88
 25  \w     35.00  79.00   0.50    0.18    --  109.23 -77.00-180.00   88
 26  \w    -34.00  22.00   0.50    0.05    --   43.20 -38.00-150.00  112
 27  \w    -84.00  -4.00   0.50    0.05    --  -43.20 111.00-135.00  160
 28  \w    -96.00 -28.00   0.50    0.18    -- -104.50 111.00-135.00  136
 29  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00-180.00   86
 30  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00-150.00   86
 31  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00 -30.00   86
 32  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00   0.00   86
 33  \w    -95.00 -30.00   0.50    0.18    -- -104.50  91.00 170.88  130
 34  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00  90.00   86
 35  \w   -132.00 -89.00   0.50    0.18    -- -104.50 -15.00 120.00   86
 36  \w   -174.00 -98.00   0.50    0.18    -- -104.50-111.00 130.00  152
;
_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      -0.0295828000
_diffrn_orient_matrix_UB_12      0.0678201000
_diffrn_orient_matrix_UB_13      0.0025304000
_diffrn_orient_matrix_UB_21      0.0092394000
_diffrn_orient_matrix_UB_22      -0.0029790000
_diffrn_orient_matrix_UB_23      0.2153886000
_diffrn_orient_matrix_UB_31      0.1460989000
_diffrn_orient_matrix_UB_32      0.0139654000
_diffrn_orient_matrix_UB_33      0.0335977000
_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  0.0340
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15792
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.551
_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    2.362
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.835
_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 bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0391P)^2^+0.9576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3020
_reflns_number_total             3303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01513g2.cif
_cod_data_source_block           daz10_cu2_auto
_cod_depositor_comments
'Adding full bibliography for 7246009--7246013.cif.'
_cod_database_code               7246013
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C72  H64  Cu4  N4  O32  '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C24(H24), C15(H15), C27(H27), C25(H25), C19(H19), C28(H28)
;
_shelx_res_checksum              96483
_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 1.185
_oxdiff_exptl_absorpt_empirical_full_min 0.901