Product Distribution from Precursor Bite Angle Variation in Multitopic Alkyne Metathesis: Evidence for a Putative Kinetic Bottleneck.
Moneypenny, 2nd, Timothy P; Yang, Anna; Walter, Nathan P.; Woods, Toby J.; Gray, Danielle L.; Zhang, Yang; Moore, Jeffrey S.; Journal of the American Chemical Society 140 (2018) 5825–5833; doi:10.1021/jacs.8b02184

data_4132183
_publ_contact_author
; 
Jeffrey S. Moore 
University of Illinois 
1327A Beckman Institute 
405 North Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Product Distribution from Precursor Bite Angle Variation in Multitopic
 Alkyne Metathesis: Evidence for a Putative Kinetic Bottleneck.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5825
_journal_page_last               5833
_journal_paper_doi               10.1021/jacs.8b02184
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         ' C39 H36 S3 '
_chemical_formula_sum            'C39 H36 S3'
_chemical_formula_weight         600.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8694(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9615(6)
_cell_length_b                   14.7481(6)
_cell_length_c                   16.6133(7)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.53
_cell_volume                     3321.0(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd58asa
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            93160
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         2.202
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  0.94943
_exptl_absorpt_correction_T_min  0.91564
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_id                dd58asa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-4 -4 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.421
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0232(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0400P)^2^+1.6269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7403
_reflns_number_total             8271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02184_si_002.cif
_cod_data_source_block           dd58asa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132183
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              32689
_shelx_hkl_checksum              94493