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_7716153
_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         'C43 H34 Dy F3 N5 O5 P'
_chemical_formula_sum            'C43 H34 Dy F3 N5 O5 P'
_chemical_formula_weight         951.22
_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             2023-12-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                88.990(3)
_cell_angle_beta                 83.329(3)
_cell_angle_gamma                62.514(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1068(6)
_cell_length_b                   11.8584(5)
_cell_length_c                   16.9438(5)
_cell_measurement_reflns_used    14102
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.6160
_cell_measurement_theta_min      3.0520
_cell_volume                     1964.70(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -15.00  35.00   0.50    1.91    --   -7.50 -82.00  90.00  100
  2  \w    -95.00  26.00   0.50    1.91    --   -7.50 -38.00  60.00  242
  3  \w    -39.00   3.00   0.50    1.91    --   -7.50 -82.00 -30.00   84
  4  \w     13.00  39.00   0.50    1.91    --   -7.50  38.00 -60.00   52
  5  \w    -94.00  10.00   0.50    1.91    --   -7.50 -38.00-150.00  208
  6  \w    -89.00  33.00   0.50    1.91    --   -7.50   0.00-180.00  244
  7  \w     56.00  81.00   0.50    1.91    --   -7.50   0.00-180.00   50
  8  \w    -96.00  -1.00   0.50    1.91    --   -7.50 -57.00   0.00  190
;
_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      0.0486021000
_diffrn_orient_matrix_UB_12      -0.0439663000
_diffrn_orient_matrix_UB_13      -0.0297188000
_diffrn_orient_matrix_UB_21      -0.0296267000
_diffrn_orient_matrix_UB_22      0.0440022000
_diffrn_orient_matrix_UB_23      -0.0296217000
_diffrn_orient_matrix_UB_31      0.0449481000
_diffrn_orient_matrix_UB_32      0.0261630000
_diffrn_orient_matrix_UB_33      0.0043210000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31017
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.500
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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    1.608
_exptl_crystal_description       needle
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.004
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0237P)^2^+2.8832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7299
_reflns_number_total             8005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00803k2.cif
_cod_data_source_block           aj0432
_cod_depositor_comments
'Adding full bibliography for 7716151--7716154.cif.'
_cod_database_code               7716153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H20N4O6Dy1F1P1
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a 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), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
2.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c)
;
_shelx_res_checksum              41937
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.786