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_1572256
_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 Al, C16 H32 Li O4'
_chemical_formula_sum            'C44 H60 Al Li O4'
_chemical_formula_weight         686.84
_chemical_name_systematic
'tetrakis(tetrahydrofuran)lithium tetrakis(o-tolyl)aluminate'
_chemical_properties_physical    Moisture-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                70.41(4)
_cell_angle_beta                 86.22(4)
_cell_angle_gamma                85.05(5)
_cell_formula_units_Z            4
_cell_length_a                   11.461(6)
_cell_length_b                   16.903(11)
_cell_length_c                   22.031(10)
_cell_measurement_reflns_used    18236
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.51
_cell_measurement_theta_min      5.50
_cell_volume                     4003(4)
_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 X-Red 2.3.0.0 (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 0.964
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
 3817 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  0.0554
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51576
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.796
_diffrn_reflns_theta_min         2.781
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.6178
_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
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method layering
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14313
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7669
_reflns_number_total             14313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03107e2.cif
_cod_data_source_block           al_otolyl_4_lithf_4
_cod_depositor_comments
'Adding full bibliography for 1572252--1572256.cif.'
_cod_database_code               1572256
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C84-C83 \\sim C84-C82
 with sigma of 0.02
 C81-C83 \\sim C81-C82
 with sigma of 0.02
3. Others
 Fixed Sof: H81A(0.5) H81B(0.5) H81C(0.5) H81D(0.5) H84A(0.5) H84B(0.5)
 H84C(0.5) H84D(0.5) C83(0.5) H83A(0.5) H83B(0.5) C82(0.5) H82A(0.5) H82B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), 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), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80A,H80B), C81(H81A,H81B), C81(H81C,H81D), C84(H84A,H84B), C84(H84C,H84D),
  C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C83(H83A,H83B), C82(H82A,H82B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), 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)
4.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              52923
_shelx_hkl_checksum              44842
_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   18.0
_stoe_evaluation_integration_b   1.0
_stoe_evaluation_integration_ems 0.046
_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 94.8
_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 139.6
_stoe_evaluation_lana_max_2theta_desired 139.6
_stoe_evaluation_lana_mean_redundancy 3.6
_stoe_evaluation_lana_number_refls_after_or 51578
_stoe_evaluation_lana_number_refls_outliers 637
_stoe_evaluation_lana_number_refls_total 52215
_stoe_evaluation_lana_number_refls_unique 14314
_stoe_evaluation_lana_number_refls_written 51578
_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          12.5   27.5   42.5   57.5   72.5   87.5  102.5  117.5  132.5
<Resolution>    5.33   3.08   2.12   1.57   1.29   1.12   1.00   0.90   0.85
N(total)         217   1403   2364   4605   8818  11604   9001   9656   4547
<Redundancy>     2.3    3.2    2.6    3.1    4.3    4.8    3.6    3.6    2.3
Complet. [%%]    91.8  100.0   99.0   98.4   98.8   98.4   91.8   96.9   83.7
<I/sigma>      106.2   55.1   19.5    8.3    4.7    3.1    2.3    1.4    1.2
R(int)         0.017  0.015  0.026  0.041  0.067  0.085  0.110  0.178  0.205
;
_stoe_measurement_identifier     Al_otolyl_4_LiTHF_4
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '4.8 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '5.1 h'
_stoe_measurement_total_frame_number 3817
_stoe_measurement_total_run_number 50
_stoe_measurement_tube_power     '50.0 W'