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_7716151
_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         'C48 H39 Dy N5 O5 P, 2[CH3OH]'
_chemical_formula_sum            'C48 H39 Dy N5 O5 P'
_chemical_formula_weight         959.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.613(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1458(6)
_cell_length_b                   22.4579(9)
_cell_length_c                   15.9855(7)
_cell_measurement_reflns_used    18971
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      28.4230
_cell_measurement_theta_min      2.8730
_cell_volume                     4545.2(4)
_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_environment      N~2~
_diffrn_ambient_temperature      120(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.890
_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     -7.00  18.00   0.50    4.54    --    7.10 -82.00  31.00   50
  2  \w    -38.00 -13.00   0.50    4.54    --   -7.50 -82.00  31.00   50
  3  \w     61.00  96.00   0.50    4.54    --    7.10  77.00   0.00   70
  4  \w     51.00  96.00   0.50    4.54    --    7.10  77.00 -60.00   90
  5  \w     -4.00  35.00   0.50    4.54    --   -7.50 -82.00  90.00   78
  6  \w    -63.00  -9.00   0.50    4.54    --   -7.50 -77.00 -30.00  108
  7  \w    -39.00 -11.00   0.50    4.54    --   -7.50 -82.00 -60.00   56
  8  \w      8.00  33.00   0.50    4.54    --   -7.50 -82.00 -60.00   50
  9  \w    -52.00  34.00   0.50    4.54    --   -7.50 -82.00-180.00  172
 10  \w    -48.00 -14.00   0.50    4.54    --   -7.50 -82.00  90.00   68
;
_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      -0.0339483000
_diffrn_orient_matrix_UB_12      0.0017372000
_diffrn_orient_matrix_UB_13      0.0277062000
_diffrn_orient_matrix_UB_21      0.0204514000
_diffrn_orient_matrix_UB_22      -0.0273752000
_diffrn_orient_matrix_UB_23      0.0195241000
_diffrn_orient_matrix_UB_31      0.0396370000
_diffrn_orient_matrix_UB_32      0.0156035000
_diffrn_orient_matrix_UB_33      0.0312376000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49949
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.960
_diffrn_reflns_theta_min         2.424
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39424
_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    1.402
_exptl_crystal_description       needle
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10709
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.1058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8673
_reflns_number_total             10709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00803k2.cif
_cod_data_source_block           aj0427
_cod_depositor_comments
'Adding full bibliography for 7716151--7716154.cif.'
_cod_database_code               7716151
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H20N4O6Dy1P1
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.625
_reflns_odcompleteness_completeness 99.67
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C49 \\sim C18-C23
 with sigma of 0.02
 C20-C51 \\sim C20-C22
 with sigma of 0.02
 C49-C50 \\sim C23-C21
 with sigma of 0.02
 C51-C50 \\sim C22-C21
 with sigma of 0.02
 C49-C51 \\sim C23-C22
 with sigma of 0.04
 C18-C50 \\sim C18-C21
 with sigma of 0.04
 C20-C50 \\sim C20-C21
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C23)=Sof(H23)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(H20a)=1-FVAR(1)
 Sof(H20)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C23(H23), C21(H21), C22(H22), C20(H20), C20(H20a),
 C19(H19), C17(H17), C16(H16), C15(H15), C14(H14), C13(H13), C36(H36), C35(H35),
  C34(H34), C33(H33), C32(H32), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C42(H42), C41(H41), C40(H40), C39(H39), C38(H38), C49(H49), C50(H50),
  C51(H51), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
5.b Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C11(H11a,H11b,H11c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 136 electrons were 
found in a volume of 524\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH3OH] per formula unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46038
_shelx_fab_checksum              59451
_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 2.006
_oxdiff_exptl_absorpt_empirical_full_min 0.430