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_4132185
_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         'C66 H66 O3'
_chemical_formula_sum            'C66 H66 O3'
_chemical_formula_weight         907.18
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   15.2838(10)
_cell_length_b                   15.2838(10)
_cell_length_c                   27.2130(19)
_cell_measurement_reflns_used    9474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.67
_cell_volume                     5505.2(6)
_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, 
(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 0.996
_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  dd53as_sq
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            79503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.438
_diffrn_reflns_theta_min         2.665
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1944
_exptl_crystal_id                dd53as_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research). 
;
_platon_squeeze_details
; 
Significant electron density was removed from six identified void spaces. 
The removed electron density is slightly below that expected for methanol 
molecules; this slight underestimation is most likely a result of the low 
resolutoin of the collected diffraction data. The most probable solution 
is one that includes six methanol molecules per unit cell. 
;
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0069(5)
_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   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3392
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.1176
_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^)+(0.0100P)^2^+21.7630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3217
_reflns_number_total             3392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02184_si_002.cif
_cod_data_source_block           dd53as_sq
_cod_original_cell_volume        5505.2(8)
_cod_database_code               4132185
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              3306
_shelx_hkl_checksum              92963
_shelx_fab_checksum              97580
_platon_squeeze_void_probe_radius 1.20