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_7245769
_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
'C39 H25 Dy2 N19 O11,2(C3 H7 N O), (C H4 O), 2(H2 O)'
_chemical_formula_sum            'C46 H47 Dy2 N21 O16'
_chemical_formula_weight         1475.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 101.8928(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.56781(18)
_cell_length_b                   12.14163(10)
_cell_length_c                   23.5494(2)
_cell_measurement_reflns_used    21426
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6220
_cell_measurement_theta_min      3.6140
_cell_volume                     6314.26(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 0.997
_diffrn_measured_fraction_theta_max 0.970
_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  -2.00   0.50    0.80    --  -46.93 108.00 -44.00  100
  2  \w     14.00  81.00   0.50    0.80    --   46.93-108.00-141.00  134
  3  \w    -78.00 -52.00   0.50    3.20    --  -99.00 108.00 -44.00   52
  4  \w   -139.00 -94.00   0.50    3.20    --  -99.00-108.00-141.00   90
  5  \w     89.00 151.00   0.50    3.20    --   99.00 108.00 -44.00  124
  6  \w     43.00  68.00   0.50    3.20    --   99.00-108.00-141.00   50
  7  \w    -20.00  29.00   0.50    0.80    --  -46.93  19.00  90.00   98
  8  \w    -24.00  26.00   0.50    0.80    --  -46.93  57.00 120.00  100
  9  \w    -14.00  12.00   0.50    0.80    --  -46.93  19.00 -30.00   52
 10  \w     -2.00  25.00   0.50    0.80    --   46.93 -57.00   0.00   54
 11  \w    -17.00  18.00   0.50    0.80    --   46.93 -19.00 120.00   70
 12  \w   -104.00 -28.00   0.50    3.20    --  -99.00  77.00  60.00  152
 13  \w    -69.00 -44.00   0.50    3.20    --  -99.00  61.00 150.00   50
 14  \w   -166.00 -87.00   0.50    3.20    --  -99.00 -30.00 -60.00  158
 15  \w    -69.00 -27.00   0.50    3.20    --  -99.00  61.00  30.00   84
 16  \w   -173.00 -92.00   0.50    3.20    --  -99.00 -15.00  60.00  162
 17  \w    -69.00 -29.00   0.50    3.20    --  -99.00  61.00 -60.00   80
 18  \w   -109.00 -26.00   0.50    3.20    --  -99.00 125.00 120.00  166
 19  \w     27.00  52.00   0.50    3.20    --   99.00 -45.00 120.00   50
 20  \w     35.00  66.00   0.50    3.20    --   99.00 -61.00  30.00   62
 21  \w     27.00  53.00   0.50    3.20    --   99.00 -61.00   0.00   52
 22  \w     34.00  59.00   0.50    3.20    --   99.00 -61.00  90.00   50
 23  \w     29.00  70.00   0.50    3.20    --   99.00 -61.00 -90.00   82
 24  \w     26.00  68.00   0.50    3.20    --   99.00 -61.00-150.00   84
 25  \w     28.00  53.00   0.50    3.20    --   99.00 -45.00 -60.00   50
 26  \w     28.00  53.00   0.50    3.20    --   99.00 -45.00  90.00   50
 27  \w     27.00  52.00   0.50    3.20    --   99.00 -45.00   0.00   50
;
_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      -0.0423391000
_diffrn_orient_matrix_UB_12      -0.0985047000
_diffrn_orient_matrix_UB_13      0.0028181000
_diffrn_orient_matrix_UB_21      0.0277915000
_diffrn_orient_matrix_UB_22      -0.0139399000
_diffrn_orient_matrix_UB_23      0.0650744000
_diffrn_orient_matrix_UB_31      -0.0479702000
_diffrn_orient_matrix_UB_32      0.0786716000
_diffrn_orient_matrix_UB_33      0.0151810000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.594
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46970
_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    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.526
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+20.5138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11163
_reflns_number_total             12343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01303g2.cif
_cod_data_source_block           0318-8zyj_auto_sq
_cod_original_cell_volume        6314.26(10)
_cod_database_code               7245769
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Dy'
_shelx_estimated_absorpt_t_max   0.352
_shelx_estimated_absorpt_t_min   0.110
_diffrn_oxdiff_digest_frames
;
01f9996a8f53ac6d892314d727ad199ecf00035e899
;
_diffrn_oxdiff_digest_hkl
;
01b36b12fa1717f439bc8cf7a4b09194e0af96
;
_reflns_odcompleteness_completeness 99.77
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N16(H16), C0AA(H0AA), C17(H17), C29(H29), C5(H5), C5AA(H5AA),
 C21(H21), C34(H34), C1AA(H1AA), C31(H31), C7(H7), C10(H10), C32(H32), C33(H33),
  C8(H8A), C9(H9)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              72030
_shelx_hkl_checksum              40620
_shelx_fab_checksum              55599
_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 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.673