Slow magnetic relaxation in a homoaxially phosphine oxide coordinated pentagonal bipyramidal Dy(III) complex.
Kalita, Pankaj; Ahmed, Naushad; Moorthy, Shruti; Béreau, Virginie; Bar, Arun Kumar; Kumar, Pawan; Nayak, Prakash; Sutter, Jean-Pascal; Singh, Saurabh Kumar; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2804–2815; doi:10.1039/d2dt03789k

data_7712181
_publ_section_title
;
 Slow magnetic relaxation in a homoaxially phosphine oxide coordinated
 pentagonal bipyramidal Dy(III) complex.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2804
_journal_page_last               2815
_journal_paper_doi               10.1039/d2dt03789k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C59 H85 Dy N5 O4 P2, C24 H20 B'
_chemical_formula_sum            'C83 H105 B Dy N5 O4 P2'
_chemical_formula_weight         1471.96
_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             2020-06-25
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2022-07-21 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.3110(10)
_cell_angle_beta                 71.1960(10)
_cell_angle_gamma                89.0170(10)
_cell_formula_units_Z            2
_cell_length_a                   13.8161(2)
_cell_length_b                   15.6888(2)
_cell_length_c                   19.0034(3)
_cell_measurement_reflns_used    32507
_cell_measurement_temperature    297.26(10)
_cell_measurement_theta_max      28.6880
_cell_measurement_theta_min      2.3990
_cell_volume                     3898.62(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.26(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -28.00  -2.00   0.50    5.34    --    7.20 -57.00  60.00   52
  2  \w     24.00  50.00   0.50    5.34    --    7.20  57.00 -60.00   52
  3  \w     54.00  81.00   0.50    5.34    --    7.20  77.00  30.00   54
  4  \w    -49.00  35.00   0.50    5.34    --    7.20 -77.00 150.00  168
  5  \w    -23.00  31.00   0.50    5.34    --    7.20  57.00 150.00  108
  6  \w    -79.00 -53.00   0.50    5.34    --    7.20 -57.00  60.00   52
  7  \w    -48.00  51.00   0.50    5.34    --    7.20 -82.00 -90.00  198
  8  \w    -21.00   5.00   0.50    5.34    --    7.20 -82.00 -60.00   52
  9  \w     22.00  48.00   0.50    5.34    --    7.20 -82.00 -60.00   52
 10  \w    -19.00   7.00   0.50    5.34    --    7.20  57.00 -60.00   52
 11  \w    -74.00  10.00   0.50    5.34    --   -7.60 -77.00 -30.00  168
 12  \w    -56.00  -9.00   0.50    5.34    --   -7.60 -82.00  30.00   94
 13  \w    -59.00  26.00   0.50    5.34    --   -7.60 -82.00 120.00  170
 14  \w    -45.00 -20.00   0.50    5.34    --   -7.60  38.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0137646000
_diffrn_orient_matrix_UB_12      0.0026095000
_diffrn_orient_matrix_UB_13      0.0392464000
_diffrn_orient_matrix_UB_21      -0.0522591000
_diffrn_orient_matrix_UB_22      0.0039472000
_diffrn_orient_matrix_UB_23      0.0026032000
_diffrn_orient_matrix_UB_31      -0.0046205000
_diffrn_orient_matrix_UB_32      -0.0449701000
_diffrn_orient_matrix_UB_33      0.0027778000
_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  0.1065
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61931
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.201
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1542
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         14453
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+1.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12676
_reflns_number_total             14453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03789k2.cif
_cod_data_source_block           aj1105_r
_cod_depositor_comments          'Adding full bibliography for 7712181.cif.'
_cod_database_code               7712181
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOPDyB
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.591
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-C25 \\sim C24-C9A
 with sigma of 0.02
 C28-C27 \\sim C28-C5A
 with sigma of 0.02
 C27-C26 \\sim C5A-C8A
 with sigma of 0.02
 C27-C25 \\sim C5A-C9A
 with sigma of 0.04
 C25-C26 \\sim C9A-C8A
 with sigma of 0.02
 C24-C26 \\sim C24-C8A
 with sigma of 0.04
 C28-C26 \\sim C28-C8A
 with sigma of 0.04
 C37-C38 \\sim C7A-C10A
 with sigma of 0.02
 C36-C37 \\sim C36-C7A
 with sigma of 0.02
 C39-C41 \\sim C11A-C12A
 with sigma of 0.04
 C37-C39 \\sim C7A-C11A
 with sigma of 0.04
 C36-C41 \\sim C36-C12A
 with sigma of 0.02
 C38-C40 \\sim C10A-C13A
 with sigma of 0.04
 C36-C40 \\sim C36-C13A
 with sigma of 0.04
 C38-C39 \\sim C10A-C11A
 with sigma of 0.02
 C39-C40 \\sim C11A-C13A
 with sigma of 0.02
 C41-C40 \\sim C12A-C13A
 with sigma of 0.02
 C36-C38 \\sim C36-C10A
 with sigma of 0.04
 C54-C59 \\sim C54-C6A
 with sigma of 0.02
 C56-C57 \\sim C56-C15A
 with sigma of 0.02
 C54-C58 \\sim C54-C14A
 with sigma of 0.04
 C56-C58 \\sim C56-C14A
 with sigma of 0.04
 C57-C59 \\sim C15A-C6A
 with sigma of 0.04
 C57-C58 \\sim C15A-C14A
 with sigma of 0.02
 C59-C58 \\sim C6A-C14A
 with sigma of 0.02
 C39-C40 \\sim C41-C36 \\sim C37-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C27)
Uanis(C13A) = Uanis(C40)
Uanis(C10A) = Uanis(C38)
Uanis(C11A) = Uanis(C39)
4. Rigid body (RIGU) restrains
 C24, C25, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5A, C8A, C9A, C24, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7A, C10A, C11A, C12A, C13A, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6A, C14A, C15A, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H24A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(C11A)=
 Sof(H11D)=Sof(H11E)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=
 Sof(H13B)=Sof(H36A)=1-FVAR(2)
 Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 FVAR(2)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(H54A)=Sof(H56C)=Sof(H56D)=1-FVAR(3)
 Sof(H54)=Sof(H56A)=Sof(H56B)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C24(H24A), C24(H24), C30(H30), C36(H36A), C36(H36), C42(H42), C48(H48),
 C54(H54), C54(H54A)
6.b Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,
 H9AB), C10A(H10D,H10E), C11A(H11D,H11E), C12A(H12A,H12B), C13A(H13A,H13B),
 C14A(H14A,H14B), C15A(H15A,H15B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C28(H28C,H28D), C29(H29A,H29B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C55(H55A,H55B), C56(H56A,H56B), C56(H56C,H56D), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71),
 C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C79(H79), C80(H80), C81(H81),
  C82(H82), C83(H83)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              70028
_shelx_hkl_checksum              29103
_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 1.791
_oxdiff_exptl_absorpt_empirical_full_min 0.647