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_7245768
_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
'C36 H18 Dy N18 O9, 3(C6 H16 N), 2(H2 O), 3(H2 O)'
_chemical_formula_sum            'C54 H76 Dy N21 O14'
_chemical_formula_weight         1405.85
_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             2022-09-08
_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                75.5730(10)
_cell_angle_beta                 81.5450(10)
_cell_angle_gamma                73.268(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5498(2)
_cell_length_b                   14.6671(2)
_cell_length_c                   17.4729(3)
_cell_measurement_reflns_used    29848
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3860
_cell_measurement_theta_min      2.6160
_cell_volume                     3209.98(9)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_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     83.00 171.00   0.50    0.43    --   99.00  61.00  60.00  176
  2  \w     86.00 172.00   0.50    0.43    --   99.00  88.00  88.00  172
  3  \w    103.00 171.00   0.50    0.43    --   99.00  61.00  30.00  136
  4  \w     89.00 167.00   0.50    0.43    --   99.00  45.00-180.00  156
  5  \w    -16.00  75.00   0.50    0.11    --   46.92 -88.00 -27.00  182
  6  \w     70.00 112.00   0.50    0.43    --   99.00-125.00  30.00   84
  7  \w     26.00  65.00   0.50    0.43    --   99.00-125.00 -90.00   78
  8  \w     76.00 111.00   0.50    0.43    --   99.00-125.00-150.00   70
  9  \w     26.00 104.00   0.50    0.43    --   99.00-125.00-180.00  156
 10  \w     27.00  53.00   0.50    0.43    --   99.00-125.00-150.00   52
 11  \w     72.00 112.00   0.50    0.43    --   99.00-125.00 -90.00   80
 12  \w     36.00  79.00   0.50    0.43    --   99.00 -94.00-150.00   86
 13  \w     50.00  83.00   0.50    0.43    --   99.00-125.00 -60.00   66
 14  \w     87.00 112.00   0.50    0.43    --   99.00-125.00 -60.00   50
 15  \w     33.00  98.00   0.50    0.43    --   99.00 -94.00  90.00  130
 16  \w     39.00 106.00   0.50    0.43    --   99.00 -94.00  30.00  134
 17  \w     54.00 102.00   0.50    0.43    --   99.00 -88.00 -27.00   96
 18  \w     26.00  92.00   0.50    0.43    --   99.00 -77.00 -90.00  132
 19  \w     28.00  53.00   0.50    0.43    --   99.00 -45.00-150.00   50
 20  \w     28.00  53.00   0.50    0.43    --   99.00 -45.00-180.00   50
 21  \w     31.00  71.00   0.50    0.43    --   99.00 -61.00 -30.00   80
 22  \w     37.00  63.00   0.50    0.43    --   99.00 -61.00 150.00   52
 23  \w    -11.00  29.00   0.50    0.11    --  -46.92  19.00-150.00   80
 24  \w    -24.00  25.00   0.50    0.11    --  -46.92  19.00   0.00   98
 25  \w    -23.00  14.00   0.50    0.11    --  -46.92  19.00  30.00   74
 26  \w    -37.00  24.00   0.50    0.11    --  -46.92  37.00 120.00  122
 27  \w    -48.00   0.00   0.50    0.11    --  -46.92  88.00  88.00   96
 28  \w    -57.00 -31.00   0.50    0.43    --  -99.00 108.00  82.23   52
 29  \w    -90.00 -64.00   0.50    0.43    --  -99.00  88.00  88.00   52
 30  \w   -107.00 -80.00   0.50    0.43    --  -99.00 108.00  82.23   54
 31  \w   -107.00 -30.00   0.50    0.43    --  -99.00 108.00 -53.69  154
 32  \w   -104.00 -58.00   0.50    0.43    --  -99.00  77.00 -90.00   92
 33  \w    -54.00 -28.00   0.50    0.43    --  -99.00  61.00-180.00   52
 34  \w    -79.00 -36.00   0.50    0.11    --  -46.92 -37.00  60.00   86
 35  \w   -119.00 -86.00   0.50    0.11    --  -46.92 -37.00  60.00   66
 36  \w    -68.00 -41.00   0.50    0.43    --  -99.00  61.00 150.00   54
 37  \w   -170.00-102.00   0.50    0.43    --  -99.00 -15.00  30.00  136
 38  \w   -173.00-132.00   0.50    0.43    --  -99.00 -15.00   0.00   82
 39  \w   -169.00 -87.00   0.50    0.43    --  -99.00 -88.00 -27.00  164
 40  \w   -112.00 -84.00   0.50    0.11    --  -46.92-125.00  90.00   56
 41  \w   -119.00 -75.00   0.50    0.11    --  -46.92-125.00 120.00   88
;
_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      -0.0776327000
_diffrn_orient_matrix_UB_12      0.0224257000
_diffrn_orient_matrix_UB_13      0.0709814000
_diffrn_orient_matrix_UB_21      0.0869921000
_diffrn_orient_matrix_UB_22      0.0103702000
_diffrn_orient_matrix_UB_23      0.0422721000
_diffrn_orient_matrix_UB_31      -0.0243756000
_diffrn_orient_matrix_UB_32      0.1096412000
_diffrn_orient_matrix_UB_33      -0.0389595000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44179
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.786
_diffrn_reflns_theta_min         2.620
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65923
_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    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         12616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0328P)^2^+12.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11743
_reflns_number_total             12616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01303g2.cif
_cod_data_source_block           0409-6zyj_auto_sq
_cod_database_code               7245768
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy'
_shelx_estimated_absorpt_t_max   0.546
_shelx_estimated_absorpt_t_min   0.340
_diffrn_oxdiff_digest_frames
;
0171c65252fced743ebd9ff8129cb0836a0004322e4
;
_diffrn_oxdiff_digest_hkl
;
01166f8e8a87daae75d9198294720e40876a4c
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O10(H10B,H10C), O11(H11A,H11B)
2.b Ternary CH refined with riding coordinates:
 N19(H19A), N20(H20A), N21(H21A)
2.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,
 H45B), C47(H47A,H47B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,H53B)
2.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N10(H10), N16(H16), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10A),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34)
2.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              77455
_shelx_hkl_checksum              44918
_shelx_fab_checksum              1035
_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 2.221
_oxdiff_exptl_absorpt_empirical_full_min 0.651