Mechanochemical Regulation of a Photochemical Reaction.
Hu, Xiaoran; McFadden, Molly E.; Barber, Ross W.; Robb, Maxwell J.; Journal of the American Chemical Society 140 (2018) 14073–14077; doi:10.1021/jacs.8b09628

data_4133328
_publ_section_title
;
 Mechanochemical Regulation of a Photochemical Reaction.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14073
_journal_page_last               14077
_journal_paper_doi               10.1021/jacs.8b09628
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C28 H27 N O4 S2, 0.54(H2 O), 0.5(C7 H8)'
_chemical_formula_sum            'C31.5 H32.08 N O4.54 S2'
_chemical_formula_weight         561.37
_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   mixed
_audit_creation_date             2018-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506),
 SHELXL-2017/1, and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 102.88(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.007(5)
_cell_length_b                   10.872(4)
_cell_length_c                   27.409(8)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    100
_cell_measurement_theta_max      39.08
_cell_measurement_theta_min      2.51
_cell_volume                     5521(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_data_collection
'BIS V6.2.6/2017-03-27 & APEX3_2017.3-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker-AXS, 2016)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            226805
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.480
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0944 before and 0.0586 after correction. 
The Ratio of minimum to maximum transmission is 0.9719. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2371
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         31713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.6552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25850
_reflns_number_total             31713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09628_si_002.cif
_cod_data_source_block           v18389
_cod_original_cell_volume        5522(3)
_cod_original_formula_sum        'C31.50 H32.08 N O4.54 S2'
_cod_database_code               4133328
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.935
_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, All O(H) groups, All O(H,H) groups
2. Others
 Sof(O2C)=Sof(H2CO)=Sof(N1C)=Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(C5C)=Sof(H5BC)=
 Sof(H5BD)=Sof(O5B)=Sof(H5C)=Sof(H5D)=1-FVAR(1)
 Sof(O2B)=Sof(H2BO)=Sof(N1B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=
 Sof(H5BB)=FVAR(1)
 Fixed Sof: C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 C36(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5) C40(0.5)
 H40(0.5) C41(0.5) H41(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
3.a Free rotating group:
 O5(H1,H3), O5B(H5C,H5D)
3.b Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C16(H16), C2B(H2B), C7B(H7B), C16B(H16B)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C14(H14A,H14B), C17(H17A,H17B), C4B(H4BA,H4BB),
 C5B(H5BA,H5BB), C4C(H4CA,H4CB), C5C(H5BC,H5BD), C14B(H14C,H14D), C17B(H17C,
 H17D)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C15(H15), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C8B(H8B), C15B(H15B), C22B(H22B), C24B(H24B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
3.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C12B(H12D,H12E,H12F), C20B(H20D,
 H20E,H20F), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C)
3.f Idealised tetrahedral OH refined as rotating group:
 O2(H2O), O4(H4O), O2B(H2BO), O2C(H2CO), O4B(H4BO)
;
_shelx_res_checksum              37134
_shelx_hkl_checksum              45168
_olex2_submission_special_instructions 'No special instructions were received'