Six-coordinate mononuclear dysprosium(iii) single-molecule magnets with the triphenylphosphine oxide ligand.
Vignesh, Kuduva R.; Alexandropoulos, Dimitris I.; Xie, Haomiao; Dunbar, Kim R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4694–4698; doi:10.1039/d0dt00801j

data_7703923
_publ_section_title
;
 Six-coordinate mononuclear dysprosium(iii) single-molecule magnets with
 the triphenylphosphine oxide ligand.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4694
_journal_page_last               4698
_journal_paper_doi               10.1039/d0dt00801j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C72 H59.704 Dy I2 O4 P4, 3(C4 H8 O), 0.296(H2 O), I'
_chemical_formula_sum            'C92 H100.8 Dy I3 O10.3 P4'
_chemical_formula_weight         2038.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-11 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.9660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5253(8)
_cell_length_b                   23.7303(10)
_cell_length_c                   20.0073(8)
_cell_measurement_reflns_used    9096
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.401
_cell_measurement_theta_min      2.295
_cell_volume                     8412.6(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.02
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            134635
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    2.125
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1158 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8162. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             4081
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         15503
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0297P)^2^+25.7060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14606
_reflns_number_total             15503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00801j3.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7703921--7703923.cif.'
_cod_original_formula_sum        'C92 H100.80 Dy I3 O10.30 P4'
_cod_database_code               7703923
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.676
_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 O(H,H) groups
2. Restrained distances
 C5-C6 = C7-C8
 1.53 with sigma of 0.02
 O1-C5 = O1-C8
 1.44 with sigma of 0.02
 C6-C7
 1.54 with sigma of 0.02
 C10-C11 = C13-C14
 1.53 with sigma of 0.02
 O3-C10 = O3-C14
 1.44 with sigma of 0.02
 C11-C13
 1.54 with sigma of 0.02
 O1-C6 = O1-C7 = C5-C7 = C6-C8
 2.38 with sigma of 0.04
 O3-C11 = O3-C13 = C10-C13 = C11-C14
 2.38 with sigma of 0.04
 C5-C6 \\sim C6-C7 \\sim C7-C8
 with sigma of 0.02
 O1-C5 \\sim O1-C8
 with sigma of 0.02
 O1-C6 \\sim O1-C7
 with sigma of 0.04
 C6-C8 \\sim C5-C7
 with sigma of 0.04
 O3-C11 \\sim O3-C13
 with sigma of 0.04
 O3-C10 \\sim O3-C14
 with sigma of 0.02
 C11-C14 \\sim C10-C13
 with sigma of 0.04
 C10-C11 \\sim C11-C13 \\sim C13-C14
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O3 \\sim C10 \\sim C11 \\sim C13 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C20, O2, C3, C9, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C0AA, O4, C1, C2, C9AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C10, C11, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, O3, C10, C11, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, O1, C8, C7, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O5)=Sof(H5C)=Sof(H5D)=Sof(O3)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 1-FVAR(1)
 Sof(H00Y)=Sof(O1)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(1)
 Sof(I3)=1-FVAR(2)
 Sof(I004)=FVAR(2)
6.a Free rotating group:
 C1(O4,C2,C9AA), O2(C3,C9,C12), O5(H5C,H5D)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1(H1A,H1B), C2(H2A,H2B), C9AA(H9AA,H9AB), C20(H20A,H20B),
 C3(H3A,H3B), C9(H9A,H9B), C12(H12A,H12B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,
 H14B)
6.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00L(H00L), C00N(H00N), C00O(H00O), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E),
 C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01T(H01T), C01V(H01V), C01W(H01W), C01X(H01X),
 C01Y(H01Y), C01Z(H01Z), C02A(H02A), C02B(H02B), C02C(H02C), C4(H4), C010(H010),
  C011(H011), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
 C019(H019), C020(H020), C021(H021), C022(H022), C023(H023), C024(H024),
 C025(H025), C026(H026), C027(H027), C028(H028), C029(H029)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 216 electrons were
found in a volume of 744\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 1[C4H8O] and 1[H2O]
per Formula Unit which account for 200 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68184
_shelx_fab_checksum              37839
_olex2_submission_special_instructions 'No special instructions were received'