Syntheses, structures and magnetic properties of mononuclear, dinuclear and tetranuclear dysprosium(III) complexes based on azotetrazole-3-hydroxy-2-naphthoic acid
Zhong, Yun-Jing; Zhu, Yu-Ying; Mo, Jin-Lin; Ye, Sheng-Lan; Luo, Wen-Dan; Huang, Xin; Chen, Wen-Bin; Dong, Wen; CrystEngComm  (2022) –; doi:10.1039/D2CE01303G

data_7245770
_publ_section_title
;
 Syntheses, structures and magnetic properties of mononuclear, dinuclear
 and tetranuclear dysprosium(III) complexes based on
 azotetrazole-3-hydroxy-2-naphthoic acid
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01303G
_journal_year                    2022
_chemical_formula_moiety
'C72 H40 Dy4 N36 O20, C3 H7 N O, 7(H2 O), 6(C6 H16 N), 2(C2 H3 N), (H2 O)'
_chemical_formula_sum            'C115 H165 Dy4 N45 O29'
_chemical_formula_weight         3291.91
_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
_audit_creation_date             2022-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.4820(10)
_cell_angle_beta                 76.1500(10)
_cell_angle_gamma                75.6980(10)
_cell_formula_units_Z            2
_cell_length_a                   14.5277(2)
_cell_length_b                   19.5900(3)
_cell_length_c                   24.9631(4)
_cell_measurement_reflns_used    41899
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.6080
_cell_measurement_theta_min      2.9290
_cell_volume                     6682.64(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_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   -119.00 -42.00   0.50    0.74    --  -46.92 -59.00  68.00  154
  2  \w    -54.00 -25.00   0.50    0.74    --  -46.92  59.00-151.00   58
  3  \w     34.00 117.00   0.50    0.74    --   46.92  59.00-151.00  166
  4  \w    -23.00  60.00   0.50    0.74    --   46.92 -59.00  68.00  166
  5  \w   -170.00 -84.00   0.50    2.14    --  -99.00 -59.00  68.00  172
  6  \w    -65.00 -35.00   0.50    2.14    --  -99.00  59.00-151.00   60
  7  \w     32.00  68.00   0.50    2.14    --   99.00 -59.00  68.00   72
  8  \w    130.00 171.00   0.50    2.14    --   99.00  59.00-151.00   82
  9  \w    -17.00  21.00   0.50    0.74    --  -46.92  59.00-151.00   76
 10  \w   -101.00 -74.00   0.50    0.74    --  -46.92-125.00-150.00   54
 11  \w     20.00  56.00   0.50    0.74    --   46.92-125.00-180.00   72
 12  \w     18.00  56.00   0.50    0.74    --   46.92-125.00 120.00   76
 13  \w     66.00  94.00   0.50    0.74    --   46.92-125.00 120.00   56
 14  \w    -25.00  28.00   0.50    0.74    --   46.92 -19.00 -90.00  106
 15  \w   -126.00 -92.00   0.50    2.14    --  -99.00 144.00-151.15   68
 16  \w    -81.00 -40.00   0.50    2.14    --  -99.00 144.00-151.15   82
 17  \w   -165.00 -87.00   0.50    2.14    --  -99.00 -94.00-180.00  156
 18  \w   -125.00 -99.00   0.50    2.14    --  -99.00 143.00  39.61   52
 19  \w   -156.00 -92.00   0.50    2.14    --  -99.00 -45.00  30.00  128
 20  \w   -114.00 -89.00   0.50    2.14    --  -99.00 130.00 114.65   50
 21  \w    -64.00 -27.00   0.50    2.14    --  -99.00  61.00  60.00   74
 22  \w   -108.00 -33.00   0.50    2.14    --  -99.00 110.00 168.83  150
 23  \w   -103.00 -28.00   0.50    2.14    --  -99.00  77.00 -30.00  150
 24  \w   -108.00 -82.00   0.50    2.14    --  -99.00 111.00 -31.44   52
 25  \w   -116.00 -79.00   0.50    2.14    --  -99.00 132.00  -5.22   74
 26  \w    -79.00 -53.00   0.50    2.14    --  -99.00 143.00  39.61   52
 27  \w    -75.00 -29.00   0.50    2.14    --  -99.00 111.00 -31.44   92
 28  \w    -84.00 -26.00   0.50    2.14    --  -99.00 130.00 114.65  116
 29  \w     86.00 151.00   0.50    2.14    --   99.00  45.00-120.00  130
 30  \w     83.00 109.00   0.50    2.14    --   99.00-125.00-180.00   52
 31  \w     67.00 107.00   0.50    2.14    --   99.00-125.00-120.00   80
 32  \w    102.00 169.00   0.50    2.14    --   99.00  61.00-120.00  134
 33  \w     79.00 170.00   0.50    2.14    --   99.00 125.00-120.00  182
 34  \w     30.00  74.00   0.50    2.14    --   99.00 -94.00 -60.00   88
 35  \w     75.00 107.00   0.50    2.14    --   99.00 -77.00  30.00   64
 36  \w     99.00 170.00   0.50    2.14    --   99.00  15.00 -30.00  142
 37  \w     27.00  53.00   0.50    2.14    --   99.00 -77.00  30.00   52
 38  \w     54.00 101.00   0.50    2.14    --   99.00-125.00  90.00   94
 39  \w     35.00  60.00   0.50    2.14    --   99.00 -94.00-180.00   50
 40  \w     39.00  91.00   0.50    2.14    --   99.00-125.00 -90.00  104
 41  \w     88.00 147.00   0.50    2.14    --   99.00  45.00-180.00  118
 42  \w     64.00 103.00   0.50    2.14    --   99.00-125.00   0.00   78
 43  \w     31.00  56.00   0.50    2.14    --   99.00-125.00   0.00   50
 44  \w     48.00 113.00   0.50    2.14    --   99.00-133.00  48.18  130
 45  \w     42.00  69.00   0.50    2.14    --   99.00 -61.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0907912000
_diffrn_orient_matrix_UB_12      -0.0241020000
_diffrn_orient_matrix_UB_13      0.0332465000
_diffrn_orient_matrix_UB_21      0.0370118000
_diffrn_orient_matrix_UB_22      -0.0709701000
_diffrn_orient_matrix_UB_23      -0.0296833000
_diffrn_orient_matrix_UB_31      0.0549331000
_diffrn_orient_matrix_UB_32      -0.0311678000
_diffrn_orient_matrix_UB_33      0.0453366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94700
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.965
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.505
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             3332
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.011
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         26062
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0470P)^2^+78.3397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21556
_reflns_number_total             26062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01303g2.cif
_cod_data_source_block           yunjin-sihe_auto_sq
_cod_database_code               7245770
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy'
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.212
_diffrn_oxdiff_digest_frames
;
01efbdf37748321eec5f5e722b38a1fba600033fdac
;
_diffrn_oxdiff_digest_hkl
;
013554f631b8313cff5c9dce7cd8d972435c88
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H25A,H25B} of O25A, {H25C,H25D} of O25B, All C(H,H)
  groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H19A,H19B} of O19, {H20A,H20B} of O20, {H22A,H22B} of
  O22, {H23A,H23B} of O23, {H24A,H24B} of O24, {H26A,H26B} of O26, {H27A,H27B}
  of O27, {H29A,H29B} of O29, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N45-C118
 2.6 with sigma of 0.02
 N45-C119
 1.15 with sigma of 0.02
 C119-C118
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N45 \\sim C119 \\sim C118: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C108) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O25B) \\sim Ueq, Uanis(O25A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O27) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(N44) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C119) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(N45) \\sim Ueq: with sigma
of 0.00001 and sigma for terminal atoms of 0.00002
4. Others
 Fixed Sof: O25A(0.5) H25A(0.5) H25B(0.5) O25B(0.5) H25C(0.5) H25D(0.5)
 H39(0.5) H39A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
 H10G(0.5) H10H(0.5) H10I(0.5) H10J(0.5) H10K(0.5) H10L(0.5) C112(0.5)
 H11A(0.5) H11B(0.5) H11C(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C105(0.5)
 H10M(0.5) H10N(0.5) C107(0.5) H10O(0.5) H10P(0.5) C110(0.5) H11D(0.5)
 H11E(0.5) C104(0.5) H10Q(0.5) H10R(0.5) C108(0.5) H10S(0.5) H10T(0.5)
 C111(0.5) H11F(0.5) H11G(0.5)
5.a Riding coordinates:
 O19(H19A,H19B), O25A(H25A,H25B), O25B(H25C,H25D), O26(H26A,H26B), O27(H27A,
 H27B), O29(H29A,H29B), C80(H80A,H80B,H80C), C83(H83A,H83B), C118(H11Q,H11R,
 H11S)
5.b Free rotating group:
 O22(H22A,H22B), O23(H23A,H23B), O24(H24A,H24B)
5.c Rotating group:
 O20(H20A,H20B)
5.d Ternary CH refined with riding coordinates:
 N37(H37), N38(H38), N39(H39), N39(H39A), N40(H40), N41(H41A), N42(H42)
5.e Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B), C79(H79A,H79B), C81(H81A,
 H81B), C105(H10M,H10N), C107(H10O,H10P), C110(H11D,H11E), C104(H10Q,H10R),
 C108(H10S,H10T), C111(H11F,H11G), C98(H98A,H98B), C100(H10U,H10V), C102(H10Z,
 H), C92(H92A,H92B), C94(H94A,H94B), C96(H96A,H96B), C86(H86A,H86B), C88(H88A,
 H88B), C90(H90A,H90B)
5.f Aromatic/amide H refined with riding coordinates:
 N2(H2), N8(H8), N14(H14), N20(H20), N26(H26), N32(H32), C5(H5), C7(H7),
 C8(H8A), C9(H9), C10(H10), C17(H17), C19(H19), C20(H20C), C21(H21), C22(H22),
 C29(H29), C31(H31), C32(H32A), C33(H33), C34(H34), C41(H41), C43(H43),
 C44(H44), C45(H45), C46(H46), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58),
  C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C113(H113)
5.g Idealised Me refined as rotating group:
 C114(H11H,H11I,H11J), C115(H11K,H11L,H11M), C74(H74A,H74B,H74C), C76(H76A,
 H76B,H76C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C85(H85A,H85B,H85C),
 C106(H10A,H10B,H10C), C106(H10D,H10E,H10F), C109(H10G,H10H,H10I), C109(H10J,
 H10K,H10L), C112(H11A,H11B,H11C), C1A(H1AA,H1AB,H1AC), C99(H99A,H99B,H99C),
 C101(H10W,H10X,H10Y), C103(H0AA,HA,HB), C93(H93A,H93B,H93C), C95(H95A,H95B,
 H95C), C97(H97A,H97B,H97C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C), C91(H91A,
 H91B,H91C), C117(H11N,H11O,H11P)
;
_shelx_res_checksum              4147
_shelx_hkl_checksum              76957
_shelx_fab_checksum              26139
_platon_squeeze_void_probe_radius 1.20
_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 2.753
_oxdiff_exptl_absorpt_empirical_full_min 0.144