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_4125474
_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         'C10 H12 O S8 V, 2(C24 H20 P), 2(C2 H3 N)'
_chemical_formula_sum            'C62 H58.49 N2 O P2 S8 V'
_chemical_formula_weight         1216.95
_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                103.838(10)
_cell_angle_beta                 98.039(11)
_cell_angle_gamma                98.816(11)
_cell_formula_units_Z            2
_cell_length_a                   10.663(6)
_cell_length_b                   12.686(7)
_cell_length_c                   22.853(13)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.33
_cell_volume                     2916(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      99.93
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51771
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.745
_diffrn_reflns_theta_min         1.685
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0410 before and 0.0375 after correction. The Ratio of minimum to maximum transmission is 0.9465. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             1267
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.102
_refine_diff_density_max         2.714
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         13559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0542P)^2^+4.9806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10912
_reflns_number_total             13559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b13030_si_003.cif
_cod_data_source_block           compset
_cod_depositor_comments
'Adding full bibliography for 4125472--4125474.cif.'
_cod_database_code               4125474
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All S(H,H) groups
2. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) H7AA(0.5) H7AB(0.5)
 C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) H7BC(0.5) H7BD(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C10(H10A,H10B), C10(H10C,H10D), C2(H2A,H2B),
 C7(H7AA,H7AB), C8(H8A,H8B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C35(H35), C53(H53), C43(H43), C37(H37), C31(H31), C29(H29),
 C59(H59), C41(H41), C13(H13), C15(H15), C51(H51), C52(H52), C17(H17), C47(H47),
  C33(H33), C46(H46), C32(H32), C44(H44), C16(H16), C40(H40), C50(H50),
 C38(H38), C45(H45), C19(H19), C25(H25), C39(H39), C14(H14), C34(H34), C23(H23),
  C28(H28), C58(H58), C55(H55), C27(H27), C26(H26), C57(H57), C20(H20),
 C21(H21), C56(H56), C22(H22)
3.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C60(H60A,H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'