Coherent spin-control of <i>S</i> = 1 vanadium and molybdenum complexes.
Laorenza, Daniel W.; Mullin, Kathleen R.; Weiss, Leah R.; Bayliss, Sam L.; Deb, Pratiti; Awschalom, David D.; Rondinelli, James M.; Freedman, Danna E.; Chemical science 15 (2024) 14016–14026; doi:10.1039/d4sc03107e

data_1572255
_publ_section_title
;
 Coherent spin-control of <i>S</i> = 1 vanadium and molybdenum complexes.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              14016
_journal_page_last               14026
_journal_paper_doi               10.1039/d4sc03107e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C16 H44 Si4 V, C16 H32 Li O8'
_chemical_formula_sum            'C32 H76 Li O8 Si4 V'
_chemical_formula_weight         759.16
_chemical_name_systematic
'bis(12-crown-4)lithium tetrakis(trimethylsilylmethyl)vanadate'
_chemical_properties_physical    Moisture-sensitive,Oxygen-sensitive,Pyrophoric
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.167(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4055(2)
_cell_length_b                   21.3852(3)
_cell_length_c                   20.4877(4)
_cell_measurement_reflns_used    36131
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.2180
_cell_volume                     4420.34(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.840
_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    -50.00 -23.78   0.38   15.00    --    5.03 -40.00 -31.00   69
  2  \w     -7.00  51.14   0.38   15.00    --    5.03  40.00 122.00  153
  3  \w    -70.00   3.72   0.38   15.00    --    5.03 -19.00 120.00  194
  4  \w    -11.00  38.02   0.38   15.00    --    5.03 -99.00 -60.00  129
  5  \w    -70.00   3.72   0.38   15.00    --    5.03 -19.00-150.00  194
  6  \w    -65.00 -20.92   0.38   15.00    --    5.03 -77.00 150.00  116
  7  \w     -5.00  25.40   0.38   15.00    --    5.03  37.00-150.00   80
  8  \w     51.00  77.22   0.38   15.00    --    5.03  37.00-150.00   69
  9  \w    -23.00  21.08   0.38   15.00    --   -5.49 -99.00-150.00  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0386607000
_diffrn_orient_matrix_UB_12      0.0115696000
_diffrn_orient_matrix_UB_13      0.0310764000
_diffrn_orient_matrix_UB_21      -0.0580398000
_diffrn_orient_matrix_UB_22      0.0120587000
_diffrn_orient_matrix_UB_23      0.0077268000
_diffrn_orient_matrix_UB_31      -0.0088539000
_diffrn_orient_matrix_UB_32      -0.0286563000
_diffrn_orient_matrix_UB_33      0.0157834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66678
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.100
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method layering
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         11931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0390P)^2^+0.9894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9710
_reflns_number_total             11931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03107e2.cif
_cod_data_source_block           dwl_4_59
_cod_depositor_comments
'Adding full bibliography for 1572252--1572256.cif.'
_cod_database_code               1572255
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'V Si4 C32 Li O8 H60'
_chemical_oxdiff_usercomment     'purple needles'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.794
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C13(H13A,H13B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              13048
_shelx_hkl_checksum              13402
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.380