Heterotrimetallic {LnOVPt} complexes with antiferromagnetic Ln-V coupling and magnetic memory.
Beach, Stephanie A.; Guillet, Jesse L.; Lagueux, Sydney P.; Perfetti, Mauro; Livesay, Brooke N.; Shores, Matthew P.; Bacon, Jeffrey W.; Rheingold, Arnold L.; Arnold, Polly L.; Doerrer, Linda H.; Chemical communications (Cambridge, England) 56 (2020) 11062–11065; doi:10.1039/d0cc04334f

data_7127098
_publ_section_title
;
 Heterotrimetallic {LnOVPt} complexes with antiferromagnetic Ln-V coupling
 and magnetic memory.
;
_journal_issue                   75
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11062
_journal_page_last               11065
_journal_paper_doi               10.1039/d0cc04334f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C50 H75 Ce O8 Pt S4 V, C7 H8, 0.22(C6 H18 O Si2)'
_chemical_formula_sum            'C58.32 H86.96 Ce O8.22 Pt S4 Si0.44 V'
_chemical_formula_weight         1446.34
_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
_audit_creation_date             2020-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-19 deposited with the CCDC.	2020-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9088(2)
_cell_length_b                   23.5478(5)
_cell_length_c                   17.7553(2)
_cell_measurement_reflns_used    23319
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5980
_cell_measurement_theta_min      3.0970
_cell_volume                     6636.74(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_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    -82.00  -2.00   1.00   15.00    --  -16.68 -57.00   0.00   80
  2  \w    -85.00   1.00   1.00   15.00    --  -16.68 -37.00-180.00   86
  3  \w    -87.00 -34.00   1.00   15.00    --  -16.68-179.00 150.00   53
  4  \w    -85.00   1.00   1.00   15.00    --  -16.68 -37.00  30.00   86
  5  \w    -34.00  52.00   1.00   15.00    --  -16.68  37.00-120.00   86
  6  \w    -25.00  20.00   1.00   15.00    --  -16.68 -99.00 -90.00   45
  7  \w    -85.00   1.00   1.00   15.00    --  -16.68 -37.00  90.00   86
  8  \w    -25.00  20.00   1.00   15.00    --  -16.68 -99.00 150.00   45
  9  \w    -32.00  49.00   1.00   15.00    --  -16.68  57.00 -60.00   81
 10  \w    -32.00  49.00   1.00   15.00    --  -16.68  57.00  60.00   81
 11  \w    -34.00  52.00   1.00   15.00    --  -16.68  37.00 -60.00   86
 12  \w    -47.00  33.00   1.00   15.00    --   18.25 -57.00 -30.00   80
 13  \w    -47.00  33.00   1.00   15.00    --   18.25 -57.00-120.00   80
 14  \w    -32.00  -7.00   1.00   15.00    --  -16.68  57.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124207000
_diffrn_orient_matrix_UB_12      -0.0258805000
_diffrn_orient_matrix_UB_13      -0.0164134000
_diffrn_orient_matrix_UB_21      0.0309809000
_diffrn_orient_matrix_UB_22      0.0147257000
_diffrn_orient_matrix_UB_23      -0.0193143000
_diffrn_orient_matrix_UB_31      0.0297357000
_diffrn_orient_matrix_UB_32      -0.0045354000
_diffrn_orient_matrix_UB_33      0.0309732000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            131775
_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         25.349
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.09
_exptl_absorpt_correction_T_max  1.501
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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_density_diffrn    1.448
_exptl_crystal_description       bar
_exptl_crystal_F_000             2927
_exptl_crystal_size_max          0.561
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         12139
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0343P)^2^+17.0851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9780
_reflns_number_total             12139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04334f2.cif
_cod_data_source_block           p19013_Compound_3Ce
_cod_depositor_comments
'Adding full bibliography for 7127093--7127098.cif.'
_cod_database_code               7127098
_publcif_datablock.id            {694fec41-71de-4eec-83f8-8d899af66853}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H79 Ce1 Cl2 O7 U1'
_cell_oxdiff_length_a            15.9022(4)
_cell_oxdiff_length_b            23.5490(7)
_cell_oxdiff_length_c            17.7617(5)
_cell_oxdiff_angle_alpha         89.997(2)
_cell_oxdiff_angle_beta          93.804(2)
_cell_oxdiff_angle_gamma         89.994(2)
_cell_oxdiff_volume              6636.8(3)
_cell_oxdiff_measurement_reflns_used 23315
_oxdiff_exptl_absorpt_empirical_full_min 0.586
_oxdiff_exptl_absorpt_empirical_full_max 1.501
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_theta     25.30
_reflns_odcompleteness_iscentric 1
_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. Restrained distances
 Si1S-O1S = Si2S-O1S
 1.64 with sigma of 0.02
 C33-C0AA = C36-C33 = C5BA-C33 = C35-C33 = C6BA-C33 = C34-C33
 1.54 with sigma of 0.02
 Si2S-C6S = Si2S-C5S = Si2S-C4S = Si1S-C3S = Si1S-C2S = Si1S-C1S
 1.86 with sigma of 0.02
 Si2S-Si1S
 3.2 with sigma of 0.04
 C5S-C6S
 3.02 with sigma of 0.04
 C2S-C3S
 3.02 with sigma of 0.04
 C1S-C2S
 3.02 with sigma of 0.04
 C3S-C1S
 3.02 with sigma of 0.04
 O1S-C5S
 3.02 with sigma of 0.04
 O1S-C6S
 3.02 with sigma of 0.04
 O1S-C2S
 3.02 with sigma of 0.04
 O1S-C3S
 3.02 with sigma of 0.04
 O1S-C1S
 3.02 with sigma of 0.04
 C4S-C5S
 3.02 with sigma of 0.04
 C6S-C4S
 3.02 with sigma of 0.04
 O1S-C4S
 3.02 with sigma of 0.04
3. Rigid bond restraints
 Si1S, C1S, C3S, C2S, O1S, H1SA, H1SB, H1SC, H3SA, H3SB, H3SC, H2SA, H2SB,
 H2SC, Si2S, C4S, C5S, C6S, H5SA, H5SB, H5SC, H6SA, H6SB, H6SC
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Si1S \\sim C1S \\sim C3S \\sim C2S \\sim O1S \\sim H1SA \\sim H1SB \\sim H1SC
\\sim H3SA \\sim H3SB \\sim H3SC \\sim H2SA \\sim H2SB \\sim H2SC \\sim Si2S
\\sim C4S \\sim C5S \\sim C6S \\sim H5SA \\sim H5SB \\sim H5SC \\sim H6SA \\sim
H6SB \\sim H6SC: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O1) = Uanis(O3)
Uanis(O3A) = Uanis(O1A)
Uanis(O4) = Uanis(O2)
Uanis(O2A) = Uanis(O4A)
Uanis(C5S) = Uanis(C2S)
Uanis(C6S) = Uanis(C1S)
Uanis(Si1S) = Uanis(Si2S)
Uanis(C1BA) = Uanis(C19)
Uanis(C0AA) = Uanis(C36)
Uanis(C6BA) = Uanis(C34)
Uanis(C4S) = Uanis(C3S)
Uanis(C4S) = Uanis(C6S)
5. Rigid body (RIGU) restrains
 C54, C55, C56, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S3A)=Sof(S4A)=Sof(S1A)=Sof(S2A)=Sof(O3A)=Sof(O2A)=Sof(O1A)=Sof(O4A)=1-
 FVAR(1)
 Sof(S1)=Sof(S4)=Sof(S3)=Sof(S2)=Sof(O4)=Sof(O1)=Sof(O2)=Sof(O3)=FVAR(1)
 Fixed Sof: O6(0.64892) C18(0.64892) H18A(0.64892) H18B(0.64892) H18C(0.64892)
 C36(0.70926) H36A(0.70926) H36B(0.70926) H36C(0.70926) C14(0.64892)
 C9(0.64892) C10(0.64892) C11(0.64892) H11(0.64892) C12(0.64892) H12(0.64892)
 C13(0.64892) H13(0.64892) C34(0.70926) H34A(0.70926) H34B(0.70926)
 H34C(0.70926) C35(0.70926) H35A(0.70926) H35B(0.70926) H35C(0.70926)
 C21(0.64892) H21A(0.64892) H21B(0.64892) H21C(0.64892) C22(0.64892)
 H22A(0.64892) H22B(0.64892) H22C(0.64892) C19(0.64892) C20(0.64892)
 H20A(0.64892) H20B(0.64892) H20C(0.64892) C15(0.64892) C16(0.64892)
 H16A(0.64892) H16B(0.64892) H16C(0.64892) C17(0.64892) H17A(0.64892)
 H17B(0.64892) H17C(0.64892) Si1S(0.22006) C1S(0.22006) H1SA(0.22006)
 H1SB(0.22006) H1SC(0.22006) C3S(0.22006) H3SA(0.22006) H3SB(0.22006)
 H3SC(0.22006) C2S(0.22006) H2SA(0.22006) H2SB(0.22006) H2SC(0.22006)
 O1S(0.22006) Si2S(0.22006) C4S(0.22006) H4SA(0.22006) H4SB(0.22006)
 H4SC(0.22006) C5S(0.22006) H5SA(0.22006) H5SB(0.22006) H5SC(0.22006)
 C6S(0.22006) H6SA(0.22006) H6SB(0.22006) H6SC(0.22006) C1AA(0.35108)
 O0AA(0.35108) C3AA(0.35108) H3AA(0.35108) C6AA(0.35108) C1BA(0.35108)
 C2AA(0.35108) C5AA(0.35108) H5AA(0.35108) C4AA(0.35108) H4AA(0.35108)
 C9AA(0.35108) H9AA(0.35108) H9AB(0.35108) H9AC(0.35108) C7AA(0.35108)
 C4BA(0.35108) H4BA(0.35108) H4BB(0.35108) H4BC(0.35108) C3BA(0.35108)
 H3BA(0.35108) H3BB(0.35108) H3BC(0.35108) C8AA(0.35108) H8AA(0.35108)
 H8AB(0.35108) H8AC(0.35108) C0BA(0.35108) H0BA(0.35108) H0BB(0.35108)
 H0BC(0.35108) C2BA(0.35108) H2BA(0.35108) H2BB(0.35108) H2BC(0.35108)
 C0AA(0.29074) H0AA(0.29074) H0AB(0.29074) H0AC(0.29074) C6BA(0.29074)
 H6BA(0.29074) H6BB(0.29074) H6BC(0.29074) C5BA(0.29074) H5BA(0.29074)
 H5BB(0.29074) H5BC(0.29074)
7.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C41(H41), C27(H27), C25(H25), C39(H39), C40(H40), C11(H11),
 C12(H12), C13(H13), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C3AA(H3AA), C5AA(H5AA), C4AA(H4AA)
7.b Fitted hexagon refined as free rotating group:
 C14(C9,C10,C11,C12,C13), C54(C55,C56,C57,C58,C59)
7.c Idealised Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC)
7.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C32(H32A,H32B,H32C), C50(H50A,H50B,
 H50C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C49(H49A,H49B,H49C), C36(H36A,
 H36B,H36C), C6(H6A,H6B,H6C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C21(H21A,H21B,H21C), C4(H4A,H4B,H4C), C45(H45A,H45B,H45C),
  C48(H48A,H48B,H48C), C22(H22A,H22B,H22C), C60(H60A,H60B,H60C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC),
 C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C9AA(H9AA,H9AB,H9AC), C4BA(H4BA,H4BB,
 H4BC), C3BA(H3BA,H3BB,H3BC), C8AA(H8AA,H8AB,H8AC), C0BA(H0BA,H0BB,H0BC),
 C2BA(H2BA,H2BB,H2BC), C0AA(H0AA,H0AB,H0AC), C6BA(H6BA,H6BB,H6BC), C5BA(H5BA,
 H5BB,H5BC)
;
_shelx_res_checksum              61030
_shelx_hkl_checksum              16055
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;