Structural diversity and magnetic properties of copper(ii) quinaldinate compounds with amino alcohols
Podjed, Nina; Modec, Barbara; Clérac, Rodolphe; Rouzières, Mathieu; Alcaide, María M.; López-Serrano, Joaquín; New Journal of Chemistry 46 (2022) 6899–6920; doi:10.1039/D2NJ00296E

data_7061345
_publ_section_title
;
 Structural diversity and magnetic properties of copper(ii) quinaldinate
 compounds with amino alcohols
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6899
_journal_page_last               6920
_journal_paper_doi               10.1039/D2NJ00296E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C28 H34 Cu N4 O6'
_chemical_formula_sum            'C28 H34 Cu N4 O6'
_chemical_formula_weight         586.13
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-17 deposited with the CCDC.	2022-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                92.222(4)
_cell_angle_beta                 91.154(4)
_cell_angle_gamma                91.002(4)
_cell_formula_units_Z            1
_cell_length_a                   5.8410(3)
_cell_length_b                   9.7548(4)
_cell_length_c                   11.6529(5)
_cell_measurement_reflns_used    4388
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.0340
_cell_measurement_theta_min      3.7280
_cell_volume                     663.21(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      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4933
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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      1.00  26.00   1.00    1.00    --   38.00  90.00-174.86   25
  2  \w    -44.00 -15.00   1.00    1.00    --  -41.76 -57.00 -60.00   29
  3  \w    -82.00 -52.00   1.00    1.00    --  -41.76 -57.00 -60.00   30
  4  \w    -66.00  23.00   1.00    1.00    --  -41.76  37.00  30.00   89
  5  \w    -70.00  30.00   1.00    1.00    --  -41.76  57.00 120.00  100
  6  \w     19.00  62.00   1.00    1.00    --   41.76  37.00  60.00   43
  7  \w     23.00  94.00   1.00    1.00    --   41.76-125.00 -90.00   71
  8  \w     66.00 115.00   1.00    1.00    --   41.76  37.00  60.00   49
  9  \w     11.00  36.00   1.00    1.00    --   46.00  84.00 128.73   25
 10  \w     11.00  37.00   1.00    1.00    --   46.00  84.00-143.99   26
 11  \w     13.00  38.00   1.00    1.00    --   46.00  80.00  69.91   25
 12  \w     16.00  44.00   1.00    1.00    --   50.00  82.00 -62.73   28
 13  \w     17.00  42.00   1.00    1.00    --   50.00  80.00 156.78   25
 14  \w     16.00  41.00   1.00    1.00    --   50.00  81.00 -30.78   25
 15  \w     24.00  61.00   1.00    1.00    --   54.00  77.00 179.44   37
 16  \w     30.00  57.00   1.00    1.00    --   62.00  77.00 162.83   27
 17  \w     31.00  58.00   1.00    1.00    --   62.00  76.00   0.95   27
 18  \w     30.00  57.00   1.00    1.00    --   62.00  76.00  87.02   27
 19  \w     67.00 111.00   1.00    1.00    --   62.00  76.00  87.02   44
 20  \w     37.00  64.00   1.00    1.00    --   70.00  77.00  11.66   27
 21  \w     37.00  75.00   1.00    1.00    --   70.00  77.00  36.32   38
 22  \w     38.00  66.00   1.00    1.00    --   70.00  75.00-120.86   28
 23  \w     45.00  71.00   1.00    1.00    --   70.00  50.00 -30.71   26
 24  \w     93.00 120.00   1.00    1.00    --   70.00  77.00  11.66   27
 25  \w     41.00  89.00   1.00    1.00    --   70.00  77.00 171.65   48
 26  \w     45.00  83.00   1.00    1.00    --   74.00  68.00-137.00   38
 27  \w    100.00 129.00   1.00    1.00    --   74.00  67.00 -33.07   29
 28  \w     46.00  94.00   1.00    1.00    --   74.00  67.00 -33.07   48
 29  \w     45.00  85.00   1.00    3.00    --   78.00  77.00  94.92   40
 30  \w     57.00  86.00   1.00    3.00    --   82.00  69.00  22.35   29
 31  \w     57.00  89.00   1.00    3.00    --   86.00  71.00 135.51   32
 32  \w     59.00  85.00   1.00    3.00    --   90.00  70.00 118.88   26
 33  \w     61.00 104.00   1.00    3.00    --   90.00  64.00-149.86   43
 34  \w     62.00  93.00   1.00    3.00    --   94.00  73.00-112.73   31
 35  \w     86.00 145.00   1.00    3.00    --  109.50  45.00-120.00   59
 36  \w    138.00 171.00   1.00    3.00    --  109.50 125.00  90.00   33
 37  \w     77.00 151.00   1.00    3.00    --  109.50  77.00 150.00   74
 38  \w     84.00 117.00   1.00    3.00    --  109.50  61.00 -60.00   33
 39  \w     29.00 107.00   1.00    3.00    --  109.50 -94.00  90.00   78
 40  \w     43.00 118.00   1.00    3.00    --  109.50-125.00  60.00   75
 41  \w    122.00 178.00   1.00    3.00    --  109.50  77.00 -90.00   56
 42  \w     77.00 117.00   1.00    3.00    --  109.50  77.00 -90.00   40
 43  \w     77.00 148.00   1.00    3.00    --  109.50  77.00 -60.00   71
 44  \w    143.00 176.00   1.00    3.00    --  109.50  61.00  60.00   33
 45  \w     84.00 176.00   1.00    3.00    --  109.50  77.00-120.00   92
 46  \w    116.00 143.00   1.00    3.00    --  109.50  77.00  30.00   27
 47  \w     82.00 142.00   1.00    3.00    --  109.50  61.00  60.00   60
 48  \w     77.00 103.00   1.00    3.00    --  109.50  77.00  30.00   26
 49  \w     33.00  96.00   1.00    3.00    --  109.50 -94.00 -90.00   63
 50  \w    141.00 177.00   1.00    3.00    --  109.50  77.00 120.00   36
 51  \w     78.00 139.00   1.00    3.00    --  109.50  77.00 120.00   61
 52  \w     77.00 178.00   1.00    3.00    --  109.50  77.00 -30.00  101
 53  \w     75.00 102.00   1.00    3.00    --  109.50 -94.00  30.00   27
 54  \w    111.00 174.00   1.00    3.00    --  109.50  77.00-180.00   63
 55  \w     32.00 109.00   1.00    3.00    --  109.50 -94.00-180.00   77
 56  \w     78.00 108.00   1.00    3.00    --  109.50  77.00-180.00   30
 57  \w     79.00 178.00   1.00    3.00    --  109.50  77.00   0.00   99
 58  \w     80.00 175.00   1.00    3.00    --  109.50  61.00  90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0347063000
_diffrn_orient_matrix_UB_12      0.1186568000
_diffrn_orient_matrix_UB_13      -0.0817103000
_diffrn_orient_matrix_UB_21      0.1355436000
_diffrn_orient_matrix_UB_22      -0.0782136000
_diffrn_orient_matrix_UB_23      -0.0929357000
_diffrn_orient_matrix_UB_31      -0.2236919000
_diffrn_orient_matrix_UB_32      -0.0692130000
_diffrn_orient_matrix_UB_33      -0.0468869000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.232
_diffrn_reflns_theta_min         3.797
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17968
_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            green
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             307
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2699
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0595P)^2^+0.1726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2412
_reflns_number_total             2699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00296e2.cif
_cod_data_source_block           7a
_cod_depositor_comments
'Adding full bibliography for 7061330--7061353.cif.'
_cod_database_code               7061345
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.403
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C21-C22 \\sim C21-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C22-O2A \\sim C22A-O2
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C23-O2A \\sim C23A-O2
 with sigma of 0.04
 C21-C23 \\sim C21-C23A
 with sigma of 0.04
 C21-O2A \\sim C21-O2
 with sigma of 0.04
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C21, C22, C23, C24, O2A, C22A, C23A, C24A, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H21C)=Sof(H21D)=Sof(O2A)=Sof(H2AA)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(H21A)=Sof(H21B)=Sof(O2)=Sof(H2)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C22A(H22A)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C21(H21A,H21B), C21(H21C,H21D), C23(H23A,H23B), C23A(H23C,H23D)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O2A(H2AA)
;
_shelx_res_checksum              41348
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.997
_oxdiff_exptl_absorpt_empirical_full_min 0.386