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_4125642
_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         'C14 H12 O S12 V, 2(C24 H20 P)'
_chemical_formula_sum            'C62 H52 O P2 S12 V'
_chemical_formula_weight         1310.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.211(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.6889(13)
_cell_length_b                   14.9613(7)
_cell_length_c                   14.8859(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.606
_cell_measurement_theta_min      2.651
_cell_volume                     5982.3(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      99.94
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            76400
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.637
_diffrn_reflns_theta_min         1.933
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.8660
_exptl_absorpt_correction_T_min  0.7823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1515 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.9033.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       plate
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   0.8660
_exptl_transmission_factor_min   0.7823
_refine_diff_density_max         1.177
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.356
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.1349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+285.8676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3212
_refine_ls_wR_factor_ref         0.3219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8090
_reflns_number_total             8423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13030_si_004.cif
_cod_data_source_block           mjg153d
_cod_database_code               4125642
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: V008(0.5) O011(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00H(H00C,H00G), C00M(H00H,H00J)
3.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00F(H00F), C00I(H00I), C00K(H00K), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012),
 C013(H013), C014(H014)
;
_shelx_res_checksum              46273
_shelx_hkl_checksum              83391
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'