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_7061348
_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         'C12 H33 Cu N3 O3, 2(C10 H6 N O2)'
_chemical_formula_sum            'C32 H45 Cu N5 O7'
_chemical_formula_weight         675.27
_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                110.376(4)
_cell_angle_beta                 100.665(3)
_cell_angle_gamma                91.832(3)
_cell_formula_units_Z            8
_cell_length_a                   14.1491(5)
_cell_length_b                   21.7604(9)
_cell_length_c                   23.6679(9)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.9270
_cell_measurement_theta_min      2.5530
_cell_volume                     6676.3(5)
_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 0.861
_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    -52.00 -20.00   1.00   90.00    --   14.21 -37.00  60.00   32
  2  \w     17.00  89.00   1.00   90.00    --   14.21  37.00-120.00   72
  3  \w    -40.00  46.00   1.00   90.00    --   14.21 -77.00 120.00   86
  4  \w      6.00  52.00   1.00   90.00    --   14.21  37.00  60.00   46
  5  \w    -11.00  87.00   1.00   90.00    --   14.21  57.00 -30.00   98
  6  \w    -26.00  15.00   1.00   90.00    --  -14.52 -77.00   0.00   41
;
_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      0.0447708000
_diffrn_orient_matrix_UB_12      0.0190280000
_diffrn_orient_matrix_UB_13      0.0163017000
_diffrn_orient_matrix_UB_21      0.0225533000
_diffrn_orient_matrix_UB_22      -0.0184863000
_diffrn_orient_matrix_UB_23      -0.0240267000
_diffrn_orient_matrix_UB_31      -0.0108587000
_diffrn_orient_matrix_UB_32      0.0227737000
_diffrn_orient_matrix_UB_33      -0.0150290000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.1286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            68809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.391
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54447
_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            blue
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1654
_refine_ls_number_reflns         34714
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16450
_reflns_number_total             34714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00296e2.cif
_cod_data_source_block           10e
_cod_depositor_comments
'Adding full bibliography for 7061330--7061353.cif.'
_cod_database_code               7061348
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.871
_reflns_odcompleteness_completeness 99.89
_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, 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
 O10-H10
 0.85 with sigma of 0.01
 O11-H11A
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.01
 C102-H10
 1.906992 with sigma of 0.02
 Cu4-H10
 3.077491 with sigma of 0.02
 C112-H11A
 1.912863 with sigma of 0.02
 Cu4-H11A
 2.704114 with sigma of 0.02
 C52-H5
 1.929347 with sigma of 0.02
 Cu2-H5
 3.128236 with sigma of 0.02
 C42-H4
 1.905599 with sigma of 0.02
 Cu2-H4
 2.707278 with sigma of 0.02
 C82-H8
 1.908404 with sigma of 0.02
 Cu3-H8
 3.134538 with sigma of 0.02
 C72-H7
 1.897516 with sigma of 0.02
 Cu3-H7
 2.728809 with sigma of 0.02
 C22-H2
 1.913066 with sigma of 0.02
 Cu1-H2
 2.708558 with sigma of 0.02
 C12-H1
 1.913707 with sigma of 0.02
 Cu1-H1
 3.096232 with sigma of 0.02
 C72-C71A \\sim C72-C71
 with sigma of 0.02
 N7-C71A \\sim N7-C71
 with sigma of 0.02
 C71A-C73A \\sim C73-C71
 with sigma of 0.02
 C74-C73 \\sim C73A-C74A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) = Uanis(C71A) = Uanis(C71) = Uanis(C73A) = Uanis(C74A) = Uanis(C73)
= Uanis(C74)
4. Others
 Sof(H72C)=Sof(H72D)=Sof(C71A)=Sof(H71A)=Sof(C73A)=Sof(H73C)=Sof(H73D)=
 Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(H72A)=Sof(H72B)=Sof(C71)=Sof(H71)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=
 Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C51(H51), C61(H61), C81(H81),
 C91(H91), C101(H101), C111(H111), C121(H121), C71(H71), C71A(H71A)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N11(H11B,H11C),
 N12(H12C,H12D), C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B),
  C32(H32A,H32B), C33(H33A,H33B), C42(H42A,H42B), C43(H43A,H43B), C52(H52A,
 H52B), C53(H53A,H53B), C62(H62A,H62B), C63(H63A,H63B), C72(H72A,H72B),
 C72(H72C,H72D), C82(H82A,H82B), C83(H83A,H83B), C92(H92A,H92B), C93(H93A,H93B),
  C102(H10C,H10D), C103(H10E,H10F), C112(H11D,H11E), C113(H11F,H11G), C122(H12E,
 H12F), C123(H12G,H12H), C73(H73A,H73B), C73A(H73C,H73D)
5.c Aromatic/amide H refined with riding coordinates:
 C131(H131), C132(H132), C133(H133), C134(H134), C136(H136), C137(H137),
 C141(H141), C142(H142), C143(H143), C144(H144), C146(H146), C147(H147),
 C151(H151), C152(H152), C153(H153), C154(H154), C156(H156), C157(H157),
 C161(H161), C162(H162), C163(H163), C164(H164), C166(H166), C167(H167),
 C171(H171), C172(H172), C173(H173), C174(H174), C176(H176), C177(H177),
 C181(H181), C182(H182), C183(H183), C184(H184), C186(H186), C187(H187),
 C191(H191), C192(H192), C193(H193), C194(H194), C196(H196), C197(H197),
 C201(H201), C202(H202), C203(H203), C204(H204), C206(H206), C207(H207)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C44(H44A,H44B,
 H44C), C54(H54A,H54B,H54C), C64(H64A,H64B,H64C), C84(H84A,H84B,H84C), C94(H94A,
 H94B,H94C), C104(H10G,H10H,H10I), C114(H11H,H11I,H11J), C124(H12I,H12J,H12K),
 C74(H74A,H74B,H74C), C74A(H74D,H74E,H74F)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O9(H9), O12(H12)
;
_shelx_res_checksum              63256
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.706