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_1572254
_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 H32 Li O8, C16 H44 Al Si4'
_chemical_formula_sum            'C32 H76 Al Li O8 Si4'
_chemical_formula_weight         735.20
_chemical_name_systematic
'bis(12-crown-4)lithium tetrakis(trimethylsilylmethyl)aluminate'
_chemical_properties_physical    Moisture-sensitive
_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             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                90
_cell_angle_beta                 104.574(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4242(13)
_cell_length_b                   21.275(2)
_cell_length_c                   20.498(3)
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.00
_cell_measurement_theta_min      7.65
_cell_volume                     4399.7(10)
_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 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
 2222 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  0.0345
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33028
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.009
_diffrn_reflns_theta_min         3.046
_diffrn_source                   Axo_Cu
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_T_max  0.8542
_exptl_absorpt_correction_T_min  0.5382
_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            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_recrystallization_method layering
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0331P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0632
_reflns_d_resolution_high        0.820
_reflns_d_resolution_low         14.509
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              -19
_reflns_number_gt                5858
_reflns_number_total             8151
_reflns_threshold_expression     I>4u(I)
_cod_data_source_file            d4sc03107e2.cif
_cod_data_source_block           al_metms_4_li_12_crown_4_2
_cod_depositor_comments
'Adding full bibliography for 1572252--1572256.cif.'
_cod_original_cell_volume        4399.6(9)
_cod_database_code               1572254
_shelx_shelxl_version_number     2018/3
_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              94843
_shelx_hkl_checksum              88953
_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 0.028
_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 97.8
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 2
_stoe_evaluation_lana_max_2theta_available 140.1
_stoe_evaluation_lana_max_2theta_desired 140.1
_stoe_evaluation_lana_mean_redundancy 4.0
_stoe_evaluation_lana_number_refls_after_or 33049
_stoe_evaluation_lana_number_refls_outliers 838
_stoe_evaluation_lana_number_refls_total 33887
_stoe_evaluation_lana_number_refls_unique 8162
_stoe_evaluation_lana_number_refls_written 33049
_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 2/m
_stoe_evaluation_lana_table
;
2Theta          11.3   26.5   41.7   56.9   72.1   87.3  102.5  117.7  132.9
<Resolution>    5.63   3.20   2.16   1.59   1.29   1.12   1.00   0.90   0.85
N(total)         152   1033   2148   3378   5907   6995   5646   5782   2846
<Redundancy>     2.9    4.7    4.3    4.1    5.1    5.1    3.8    3.8    2.4
Complet. [%%]    95.7  100.0  100.0   99.9  100.0   99.9   96.3   99.9   90.8
<I/sigma>       58.2   66.3   27.2   16.0    9.1    6.5    5.4    4.8    4.3
R(int)         0.022  0.017  0.021  0.025  0.037  0.045  0.056  0.061  0.067
;
_stoe_measurement_identifier     Al_MeTMS_4_Li_12_crown_4_2
_stoe_measurement_max_exposure_per_frame '3.0 s'
_stoe_measurement_mean_exposure_per_frame '2.8 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '104 min'
_stoe_measurement_total_frame_number 2222
_stoe_measurement_total_run_number 28
_stoe_measurement_tube_power     '50.0 W'