Magnetic relaxation in two chain-like Zn2Dy2 Schiff base coordination polymers bridged by tetraoxolene and its one-electron reduced radical
Liu, Cai-Ming; Hao, Xiang; New Journal of Chemistry 45 (2021) 19868–19875; doi:10.1039/D1NJ04299H

data_7060987
_publ_section_title
;
 Magnetic relaxation in two chain-like Zn2Dy2 Schiff base coordination
 polymers bridged by tetraoxolene and its one-electron reduced radical
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19868
_journal_page_last               19875
_journal_paper_doi               10.1039/D1NJ04299H
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C53 H52 Br4 Dy2 N5 O22 Zn2, 0.5(Cl O4)'
_chemical_formula_sum            'C53 H52 Br4 Cl0.5 Dy2 N5 O24 Zn2'
_chemical_formula_weight         1936.10
_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     iterative
_audit_creation_date             2021-09-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.624(2)
_cell_angle_beta                 80.033(2)
_cell_angle_gamma                79.843(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5601(2)
_cell_length_b                   14.8370(3)
_cell_length_c                   20.0015(5)
_cell_measurement_reflns_used    32301
_cell_measurement_temperature    169.9(5)
_cell_measurement_theta_max      33.2380
_cell_measurement_theta_min      1.7040
_cell_volume                     3324.86(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_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   -105.00  65.00   0.50    6.00    --  -20.00  45.00   0.00  340
  2  \w   -105.00  65.00   0.50    6.00    --  -20.00  45.00  90.00  340
  3  \w   -105.00  65.00   0.50    6.00    --  -20.00  45.00 180.00  340
  4  \w    -97.00  73.00   0.50    6.00    --   -8.00  45.00 270.00  340
  5  \w   -125.00  45.00   0.50    6.00    --  -40.00  45.00   0.00  340
  6  \w   -125.00  45.00   0.50    6.00    --  -40.00  45.00  45.00  340
  7  \w   -125.00  45.00   0.50    6.00    --  -40.00  45.00 135.00  340
  8  \w   -125.00  45.00   0.50    6.00    --  -40.00  45.00 205.00  340
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0204413000
_diffrn_orient_matrix_UB_12      0.0017006000
_diffrn_orient_matrix_UB_13      -0.0315167000
_diffrn_orient_matrix_UB_21      0.0530234000
_diffrn_orient_matrix_UB_22      0.0146891000
_diffrn_orient_matrix_UB_23      -0.0159036000
_diffrn_orient_matrix_UB_31      0.0279029000
_diffrn_orient_matrix_UB_32      -0.0462771000
_diffrn_orient_matrix_UB_33      -0.0071406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.1198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            180466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         42.292
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             1875
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.487
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         44285
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1646
_refine_ls_R_factor_gt           0.0821
_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^+9.0706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22907
_reflns_number_total             44285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04299h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7060986--7060987.cif.'
_cod_original_cell_volume        3324.86(12)
_cod_original_formula_sum        'C53 H52 Br4 Cl0.50 Dy2 N5 O24 Zn2'
_cod_database_code               7060987
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOBrZnDy
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O17-H17
 0.85 with sigma of 0.01
 O18-H18
 0.85 with sigma of 0.01
 O22-H22
 0.85 with sigma of 0.01
 C88-H17
 1.890315 with sigma of 0.02
 Zn2-H17
 2.7107 with sigma of 0.02
 C87-H18
 1.919971 with sigma of 0.02
 Dy2-H18
 3.114065 with sigma of 0.02
 C89-H22
 1.867615 with sigma of 0.02
 Zn1-H22
 2.780913 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O25) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O26)
\\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Fixed Sof: Cl1(0.5) O25(0.5) O26(0.5) O27(0.5) O28(0.5)
5.a :
 Cl1(O25,O26,O27,O28)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C22(H22A), C23(H23), C24(H24), C27(H27), C31(H31), C33(H33), C34(H34), C35(H35)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
 H38C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99010
_shelx_fab_checksum              2441
_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 2.066
_oxdiff_exptl_absorpt_empirical_full_min 0.558