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_1572252
_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
'C28 H28 V, 0.5(C16 H32 Li O4), 0.5(C16 H31 Li O4)'
_chemical_formula_sum            'C44 H59.5 Li O4 V'
_chemical_formula_weight         710.29
_chemical_name_systematic
'tetrakis(tetrahydrofuran)lithium tetrakis(o-tolyl)vanadate'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                70.281(19)
_cell_angle_beta                 86.57(2)
_cell_angle_gamma                84.97(2)
_cell_formula_units_Z            4
_cell_length_a                   11.487(4)
_cell_length_b                   16.971(4)
_cell_length_c                   22.100(6)
_cell_measurement_reflns_used    811
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.68
_cell_measurement_theta_min      7.41
_cell_volume                     4038(2)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
 4589 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66732
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.665
_diffrn_reflns_theta_min         2.773
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.349
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1526
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Solvent layering'
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10141
_reflns_number_total             14814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03107e2.cif
_cod_data_source_block           dwl_v_otolyl_4_li_thf4
_cod_depositor_comments
'Adding full bibliography for 1572252--1572256.cif.'
_cod_original_formula_sum        'C44 H59.50 Li O4 V'
_cod_database_code               1572252
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H60,H60A,H60B} of C60, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  {H28A,H28B,H28C} of C28, {H42A,H42B,H42C} of C42, {H35A,H35B,H35C} of C35,
  {H21A,H21B,H21C} of C21, {H56A,H56B,H56C} of C56, {H49A,H49B,H49C} of C49,
  {H7A,H7B,H7C} of C7, {H14A,H14B,H14C} of C14
2. Others
 Fixed Sof: H57A(0.5) H57B(0.5) H57C(0.5) H57D(0.5) H60(0.5) H60A(0.5)
 H60B(0.5) C59(0.5) H59(0.5) C58(0.5) H58A(0.5) H58B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C57(H57C,H57D), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
  C72(H72A,H72B), C73(H73A,H73B), C58(H58A,H58B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39),
 C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C51(H51), C52(H52), C53(H53),
  C54(H54), C60(H60), C59(H59)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C)
;
_shelx_res_checksum              99006
_shelx_hkl_checksum              12122
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   13.0
_stoe_evaluation_integration_b   1.3
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 95.6
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 141.4
_stoe_evaluation_lana_max_2theta_desired 141.4
_stoe_evaluation_lana_mean_redundancy 4.5
_stoe_evaluation_lana_number_refls_after_or 66732
_stoe_evaluation_lana_number_refls_outliers 3620
_stoe_evaluation_lana_number_refls_total 70352
_stoe_evaluation_lana_number_refls_unique 14814
_stoe_evaluation_lana_number_refls_written 66732
_stoe_evaluation_lana_or_c1      0.050
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      1.0
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          12.7   27.9   43.1   58.3   73.5   88.7  103.9  119.1  134.3
<Resolution>    5.36   3.04   2.07   1.57   1.28   1.10   0.99   0.90   0.84
N(total)         482   2684   4741   8549  12694  14330  11352  10575   4945
<Redundancy>     4.2    5.4    4.6    5.3    5.7    5.5    4.1    3.8    2.5
Complet. [%%]    97.0  100.0  100.0   99.9   99.2   98.9   94.5   97.1   82.9
<I/sigma>      166.9   79.8   35.8   16.8    8.4    5.2    4.2    2.7    2.1
R(int)         0.016  0.020  0.023  0.034  0.058  0.085  0.105  0.157  0.195
;
_stoe_measurement_identifier     dwl_V_otolyl_3_norbornyl_Li_THF4_second_xta;
_stoe_measurement_max_exposure_per_frame '1.0 s'
_stoe_measurement_mean_exposure_per_frame '1.0 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '76 min'
_stoe_measurement_total_frame_number 4589
_stoe_measurement_total_run_number 68
_stoe_measurement_tube_power     '50.0 W'