Synthetic Approach To Determine the Effect of Nuclear Spin Distance on Electronic Spin Decoherence.
Graham, Michael J.; Yu, Chung-Jui; Krzyaniak, Matthew D.; Wasielewski, Michael R.; Freedman, Danna E.; Journal of the American Chemical Society 139 (2017) 3196–3201; doi:10.1021/jacs.6b13030

data_4125472
_publ_section_title
;
 Synthetic Approach To Determine the Effect of Nuclear Spin Distance on
 Electronic Spin Decoherence.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3196
_journal_page_last               3201
_journal_paper_doi               10.1021/jacs.6b13030
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C18 H12 O S16 V, 2(C24 H20 P), C4 H8 O'
_chemical_formula_sum            'C69.97 H60 O2 P2 S16 V'
_chemical_formula_weight         1558.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-19
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                92.528(3)
_cell_angle_beta                 94.167(3)
_cell_angle_gamma                108.759(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8600(7)
_cell_length_b                   13.2615(7)
_cell_length_c                   22.4444(12)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.62
_cell_volume                     3605.6(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.96
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53205
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         0.912
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.9384.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.721
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         14592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0412P)^2^+12.6077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11728
_reflns_number_total             14592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13030_si_005.cif
_cod_data_source_block           compset
_cod_depositor_comments
'Adding full bibliography for 4125472--4125474.cif.'
_cod_database_code               4125472
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C023(0.5) C026(0.5) H026(0.5) C029(0.5) H029(0.5) C02B(0.5)
 H02B(0.5) C02D(0.5) H02D(0.5) C30(0.5) H30(0.5) C02G(0.5) H02G(0.5) C02H(0.5)
 H02H(0.5) C02I(0.5) H02I(0.5) C31(0.5) H31(0.5) V1(0.25) O14(0.25) V0AA(0.75)
 O1(0.75) C9(0.5) H9(0.5) C0(0.5) C1(0.5) H1(0.5) C02K(0.5) H02K(0.5) C2(0.5)
 H2(0.5) C9A(0.5) C3(0.5) H3(0.5) C32(0.5) H32(0.5) C02J(0.5) H02J(0.5)
 C02E(0.5) H02E(0.5) C4(0.5) H4(0.5) H9A(0.5) C5(0.5) H5(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C01G(H01A,H01B), C01Q(H01C,H01D), C01R(H01E,H01F), C01U(H01G,H01H), C021(H02A,
 H02C), C022(H02L,H02M)
3.b Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00Q(H00Q), C00U(H00U), C00Y(H00Y), C010(H010), C011(H011),
 C013(H013), C014(H014), C016(H016), C018(H018), C01A(H01I), C01B(H01J),
 C01C(H01K), C01E(H01M), C01F(H01O), C01I(H01P), C01J(H01Q), C01L(H01L),
 C01N(H01N), C01O(H01R), C01P(H01S), C01S(H01T), C01T(H01U), C01V(H01V),
 C01X(H01X), C01Y(H01Y), C020(H020), C024(H024), C025(H025), C026(H026),
 C027(H027), C029(H029), C02B(H02B), C02C(H02T), C02D(H02D), C30(H30),
 C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I), C31(H31), C9(H9), C1(H1),
 C02K(H02K), C2(H2), C3(H3), C32(H32), C02J(H02J), C02E(H02E), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C028(H02N,H02O,H02P), C02A(H02Q,H02R,H02S)
;
_olex2_submission_special_instructions 'No special instructions were received'