Eight-coordinate mono- and dinuclear Dy(III) complexes containing a rigid equatorial plane and an anisobidentate carboxylate ligand in the axial position: synthesis, structure and magnetism.
Kalita, Pankaj; Kumari, Kusum; Kumar, Pawan; Kumar, Vierandra; Singh, Saurabh Kumar; Rogez, Guillaume; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10521–10535; doi:10.1039/d4dt00803k

data_7716154
_publ_section_title
;
 Eight-coordinate mono- and dinuclear Dy(III) complexes containing a rigid
 equatorial plane and an anisobidentate carboxylate ligand in the axial
 position: synthesis, structure and magnetism.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10521
_journal_page_last               10535
_journal_paper_doi               10.1039/d4dt00803k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H43 Dy N5 O5 P, [+ solvents]'
_chemical_formula_sum            'C46 H43 Dy N5 O5 P'
_chemical_formula_weight         939.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.729(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5520(7)
_cell_length_b                   19.6201(9)
_cell_length_c                   16.4532(8)
_cell_measurement_reflns_used    12693
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.0850
_cell_measurement_theta_min      2.7450
_cell_volume                     4448.8(4)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.907
_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    -25.00  49.00   0.50    5.49    --    7.10 -82.00 -90.00  148
  2  \w     51.00  96.00   0.50    5.49    --    7.10  77.00   0.00   90
  3  \w     53.00  80.00   0.50    5.49    --    7.10  77.00 150.00   54
  4  \w    -54.00 -13.00   0.50    5.49    --   -7.50 -82.00-180.00   82
  5  \w    -62.00   1.00   0.50    5.49    --   -7.50 -82.00-120.00  126
  6  \w    -91.00  22.00   0.50    5.49    --   -7.50 -57.00  30.00  226
  7  \w    -57.00   6.00   0.50    5.49    --   -7.50 -82.00   0.00  126
  8  \w    -36.00  80.00   0.50    5.49    --   -7.50  19.00 150.00  232
;
_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      0.0317363000
_diffrn_orient_matrix_UB_12      -0.0164174000
_diffrn_orient_matrix_UB_13      -0.0187248000
_diffrn_orient_matrix_UB_21      -0.0071304500
_diffrn_orient_matrix_UB_22      -0.0313438500
_diffrn_orient_matrix_UB_23      0.0185886000
_diffrn_orient_matrix_UB_31      -0.0398700500
_diffrn_orient_matrix_UB_32      -0.0074270500
_diffrn_orient_matrix_UB_33      -0.0371095000
_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  0.1009
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32964
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.008
_diffrn_reflns_theta_min         2.614
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.163
_refine_diff_density_max         4.377
_refine_diff_density_min         -2.494
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details
;
 Flack x determined using 3453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.037(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9944
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1214P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.770
_reflns_number_gt                8679
_reflns_number_total             9944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00803k2.cif
_cod_data_source_block           aj0424nw
_cod_depositor_comments
'Adding full bibliography for 7716151--7716154.cif.'
_cod_database_code               7716154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C46H43Dy1N5O5P1
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.546
_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
2. Restrained distances
 C12-C13 \\sim C12-C13A
 with sigma of 0.02
 C16-C15 \\sim C16-C15A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 C12-C14 \\sim C12-C14A
 with sigma of 0.04
 C16-C14 \\sim C16-C14A
 with sigma of 0.04
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C15A) = Uanis(C15)
Uanis(C13A) = Uanis(C13)
4. Rigid body (RIGU) restrains
 C13, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C15A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H16A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=1-FVAR(1)
 Sof(H16)=Sof(C13)=Sof(H13)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C6(H6), C46(H46), C5(H5), C19(H19), C17(H17), C23(H23), C31(H31),
 C34(H34), C22(H22), C37(H37), C32(H32), C20(H20), C33(H33), C16(H16),
 C16(H16A), C21(H21), C42(H42), C45(H45), C36(H36), C43(H43), C39(H39),
 C44(H44), C40(H40), C13(H13), C4(H4), C15(H15), C14(H14), C38(H38), C13A(H13A),
  C14A(H14A), C15A(H15A)
6.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27269
_shelx_fab_checksum              65774
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.401