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_7061349
_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         '2(C13 H15 Cu0.5 N2 O3), C3 H9 N O'
_chemical_formula_sum            'C29 H39 Cu N5 O7'
_chemical_formula_weight         633.19
_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             2021-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-12 deposited with the CCDC.	2022-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                88.622(3)
_cell_angle_beta                 76.298(4)
_cell_angle_gamma                82.897(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4853(3)
_cell_length_b                   14.1745(6)
_cell_length_c                   14.3105(6)
_cell_measurement_reflns_used    7184
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0990
_cell_measurement_theta_min      2.8310
_cell_volume                     1463.80(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.863
_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    -41.00  48.00   1.00    4.00    --   14.21 -77.00 120.00   89
  2  \w     -6.00  24.00   1.00    4.00    --  -14.52 -91.00 -14.00   30
  3  \w    -38.00 -12.00   1.00    4.00    --  -14.52  77.00 150.00   26
  4  \w    -36.00  57.00   1.00    4.00    --  -14.52  57.00   0.00   93
  5  \w    -88.00  15.00   1.00    4.00    --  -14.52 -57.00-150.00  103
;
_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      -0.0204618000
_diffrn_orient_matrix_UB_12      -0.0341386000
_diffrn_orient_matrix_UB_13      0.0368218000
_diffrn_orient_matrix_UB_21      0.0776610000
_diffrn_orient_matrix_UB_22      -0.0312936000
_diffrn_orient_matrix_UB_23      -0.0242395000
_diffrn_orient_matrix_UB_31      0.0566182000
_diffrn_orient_matrix_UB_32      0.0199571000
_diffrn_orient_matrix_UB_33      0.0256790000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.285
_diffrn_reflns_theta_min         2.822
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7569
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0480P)^2^+0.8229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6185
_reflns_number_total             7569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00296e2.cif
_cod_data_source_block           11a3a1pOH
_cod_depositor_comments
'Adding full bibliography for 7061330--7061353.cif.'
_cod_database_code               7061349
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.690
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 N5-H5B = N5-H5A
 0.89 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37)
;
_shelx_res_checksum              50469
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.687