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_4125473
_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         'C6 H12 O S4 V, 2(C24 H20 P)'
_chemical_formula_sum            'C54 H52 O P2 S4 V'
_chemical_formula_weight         958.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.969(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0523(6)
_cell_length_b                   15.3821(9)
_cell_length_c                   27.7478(16)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.635
_cell_measurement_theta_min      2.270
_cell_volume                     4714.6(5)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            99291
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         35.675
_diffrn_reflns_theta_min         1.844
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.7796
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.8477.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.598
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.309(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         37361
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.4603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                35236
_reflns_number_total             37361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13030_si_002.cif
_cod_data_source_block           mjg156c
_cod_depositor_comments
'Adding full bibliography for 4125472--4125474.cif.'
_cod_database_code               4125473
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.691(9) 0.309(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C02H(H02E,H02H), C02W(H02W,H02), C030(H03A,H03C), C034(H03D,H03E), C037(H03L,
 H03M), C038(H03F,H03G), C03A(H03H,H03I), C03C(H03N,H03O), C03D(H03P,H03Q),
 C03E(H03R,H03S), C03F(H03T,H03U), C03G(H03J,H03K)
3.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00Y(H00Y), C010(H010),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C017(H017), C019(H019), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E),
 C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01V(H01V), C01W(H01W), C01Y(H01Y), C01Z(H01Z), C020(H020),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D),
 C02F(H02F), C02G(H02G), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L),
 C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V), C02X(H02X), C02Y(H02Y),
 C02Z(H02Z), C031(H031), C032(H032), C033(H033), C035(H035), C036(H036),
 C039(H039), C03B(H03B)
;
_shelx_res_checksum              27378
_shelx_hkl_checksum              96411
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'