Kinetic Study of Living Ring-Opening Metathesis Polymerization with Third-Generation Grubbs Catalysts
Walsh, Dylan J.; Lau, Sii Hong; Hyatt, Michael G.; Guironnet, Damien; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08010

data_4126481
_publ_contact_author
; 
Damien Guironnet
University of Illinois Urbana-Champaign
Department of Chemical and Biomolecular Engineering
121 Roger Adams Laboratory MC 712
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Kinetic Study of Living Ring-Opening Metathesis Polymerization with
 Third-Generation Grubbs Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08010
_journal_year                    2017
_chemical_formula_moiety         'C33 H37 Cl2 N3 Ru'
_chemical_formula_sum            'C33 H37 Cl2 N3 Ru'
_chemical_formula_weight         647.62
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   16.3878(4)
_cell_length_b                   16.6254(4)
_cell_length_c                   22.6550(6)
_cell_measurement_reflns_used    56039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.45
_cell_volume                     6172.4(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2014)'
_computing_data_collection       'APEX3 V2016.9-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/7 (Krause et al., 2015), 
TWINABS V2012/1 (Bruker, 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  dd09hsa
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            144774
_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         26.447
_diffrn_reflns_theta_min         2.450
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.95945
_exptl_absorpt_correction_T_min  0.83109
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_id                dd09hsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
??0.3 mm cryo-loop (Hampton Research)with the (-1 5 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.096
_refine_diff_density_max         2.192
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6337
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+13.0747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5524
_reflns_number_total             6337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08010_si_002.cif
_cod_data_source_block           dd09hsa
_cod_database_code               4126481
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              82388
_shelx_hkl_checksum              41462