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_7127097
_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         'C70 H83 Ce O8 Pt S4 V, 1.5(C7 H8)'
_chemical_formula_sum            'C80.5 H95 Ce O8 Pt S4 V'
_chemical_formula_weight         1704.95
_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
_audit_creation_date             2020-06-11
_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                81.4710(10)
_cell_angle_beta                 83.2750(10)
_cell_angle_gamma                72.9520(10)
_cell_formula_units_Z            4
_cell_length_a                   16.9219(3)
_cell_length_b                   22.5655(3)
_cell_length_c                   22.5881(3)
_cell_measurement_reflns_used    28808
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0620
_cell_measurement_theta_min      3.3890
_cell_volume                     8130.3(2)
_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 2018/2 (Sheldrick, 2018)'
_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 0.999
_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    -83.00   9.00   1.00   30.00    --  -16.68 -77.00-150.00   92
  2  \w    -85.00   1.00   1.00   30.00    --  -16.68 -37.00 -90.00   86
  3  \w    -25.00  20.00   1.00   30.00    --  -16.68 -99.00  90.00   45
  4  \w    -32.00  49.00   1.00   30.00    --  -16.68  57.00  90.00   81
  5  \w    -25.00  20.00   1.00   30.00    --  -16.68 -99.00   0.00   45
  6  \w    -42.00  50.00   1.00   30.00    --  -16.68  77.00 -30.00   92
  7  \w     34.00  89.00   1.00   30.00    --   18.25 179.00-120.00   55
  8  \w     34.00  89.00   1.00   30.00    --   18.25 179.00  90.00   55
  9  \w    -76.00 -25.00   1.00   30.00    --  -16.68 136.00-155.64   51
 10  \w    -82.00  -2.00   1.00   30.00    --  -16.68 -57.00  90.00   80
 11  \w    -77.00  -5.00   1.00   30.00    --  -16.68 137.00 108.77   72
 12  \w     -2.00  72.00   1.00   30.00    --   18.25-127.00  33.56   74
 13  \w      3.00  84.00   1.00   30.00    --   18.25  57.00  60.00   81
 14  \w    -50.00  36.00   1.00   30.00    --   18.25 -37.00-150.00   86
;
_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      -0.0304106000
_diffrn_orient_matrix_UB_12      0.0214188000
_diffrn_orient_matrix_UB_13      -0.0176891000
_diffrn_orient_matrix_UB_21      -0.0150285000
_diffrn_orient_matrix_UB_22      -0.0248232000
_diffrn_orient_matrix_UB_23      -0.0052808000
_diffrn_orient_matrix_UB_31      -0.0279872000
_diffrn_orient_matrix_UB_32      0.0046689000
_diffrn_orient_matrix_UB_33      0.0259536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            173635
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.532
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7068
_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    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             3460
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.033
_platon_squeeze_details
;
Spek, A.L. (2015). <i>PLATON SQUEEZE: a tool for the calculation of the disordered solvent
contribution to the calculated structure factors</i>. Acta Cryst. C<b>71</b>, 9
 - 18.
;
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         33218
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0349P)^2^+7.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23397
_reflns_number_total             33218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04334f2.cif
_cod_data_source_block           p19016_Compound_4Ce
_cod_depositor_comments
'Adding full bibliography for 7127093--7127098.cif.'
_cod_original_formula_sum        'C80.50 H95 Ce O8 Pt S4 V'
_cod_database_code               7127097
_publcif_datablock.id            {e931198c-b920-4f98-9778-326379fa4144}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C70 O8 S4 H68 V1 Pt1 Ce1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_platon_squeeze_void_probe_radius 1.20
_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
 V1-O3A \\sim V1-O3B
 with sigma of 0.02
 V1-O2A \\sim V1-O2B
 with sigma of 0.02
 V1-O4A \\sim V1-O4B
 with sigma of 0.02
 V1-O1A \\sim V1-O1B
 with sigma of 0.02
 Pt1-S4A \\sim Pt1-S4B
 with sigma of 0.02
 Pt1-S1B \\sim Pt1-S1A
 with sigma of 0.02
 Pt1-S2B \\sim Pt1-S2A
 with sigma of 0.02
 Pt1-S3B \\sim Pt1-S3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S3A) = Uanis(S3B)
Uanis(O2B) = Uanis(O4B)
4. Others
 Sof(O3A)=Sof(O4A)=Sof(O2A)=Sof(O1A)=Sof(S3A)=Sof(S2A)=Sof(S4A)=Sof(S1A)=1-
 FVAR(1)
 Sof(S1B)=Sof(S2B)=Sof(S4B)=Sof(S3B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C87(H87), C59(H59), C101(H101), C7(H7), C94(H94), C91(H91), C28(H28),
 C45(H45), C60(H60), C3(H3), C88(H88), C10(H10), C47(H47), C21(H21), C117(H117),
  C33(H33), C115(H115), C27(H27), C98(H98), C84(H84), C77(H77), C46(H46),
 C73(H73), C156(H156), C6(H6), C19(H19), C61(H61), C4(H4), C160(H160), C14(H14),
  C96(H96), C89(H89), C5(H5), C26(H26), C12(H12), C17(H17), C90(H90), C11(H11),
 C116(H116), C24(H24), C32(H32), C31(H31), C103(H103), C75(H75), C76(H76),
 C74(H74), C102(H102), C83(H83), C20(H20), C95(H95), C18(H18), C97(H97),
 C142(H142), C82(H82), C158(H158), C80(H80), C131(H131), C13(H13), C129(H129),
 C157(H157), C159(H159), C143(H143), C149(H149), C130(H130), C146(H146),
 C152(H152), C81(H81), C25(H25), C150(H150), C153(H153), C144(H144), C151(H151),
  C145(H145)
5.b Idealised Me refined as rotating group:
 C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C55(H55A,H55B,H55C), C65(H65A,
 H65B,H65C), C108(H10A,H10B,H10C), C52(H52A,H52B,H52C), C64(H64A,H64B,H64C),
 C126(H12G,H12H,H12I), C140(H14A,H14B,H14C), C37(H37A,H37B,H37C), C66(H66A,H66B,
 H66C), C51(H51A,H51B,H51C), C40(H40A,H40B,H40C), C125(H12J,H12K,H12L),
 C68(H68A,H68B,H68C), C106(H10D,H10E,H10F), C54(H54A,H54B,H54C), C69(H69A,H69B,
 H69C), C41(H41A,H41B,H41C), C70(H70A,H70B,H70C), C107(H10G,H10H,H10I),
 C36(H36A,H36B,H36C), C112(H11A,H11B,H11C), C124(H12M,H12N,H12O), C42(H42A,H42B,
 H42C), C50(H50A,H50B,H50C), C139(H13A,H13B,H13C), C120(H12P,H12Q,H12R),
 C111(H11D,H11E,H11F), C136(H13D,H13E,H13F), C134(H13G,H13H,H13I), C38(H38A,
 H38B,H38C), C56(H56A,H56B,H56C), C161(H16A,H16B,H16C), C138(H13J,H13K,H13L),
 C110(H11G,H11H,H11I), C135(H13M,H13N,H13O), C154(H15A,H15B,H15C), C147(H14D,
 H14E,H14F)
;
_shelx_res_checksum              53747
_shelx_hkl_checksum              92432
_shelx_fab_checksum              85842
_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 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.747
_publcif_funding_html
;
;