Living Polymerization Caught in the Act: Direct Observation of an Arrested Intermediate in Metathesis Polymerization.
Song, Jung-Ah; Park, Bohyun; Kim, Soohyung; Kang, Cheol; Lee, Dongwhan; Baik, Mu-Hyun; Grubbs, Robert H.; Choi, Tae-Lim; Journal of the American Chemical Society 141 (2019) 10039–10047; doi:10.1021/jacs.9b04019

data_4128267
_publ_section_title
;
 Living Polymerization Caught in the Act: Direct Observation of an
 Arrested Intermediate in Metathesis Polymerization.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10039
_journal_page_last               10047
_journal_paper_doi               10.1021/jacs.9b04019
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C64 H60 Br2 Cl2 N4 O4 Ru'
_chemical_formula_sum            'C64 H60 Br2 Cl2 N4 O4 Ru'
_chemical_formula_weight         1280.95
_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     dual
_audit_creation_date             2018-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                85.6500(10)
_cell_angle_beta                 78.0250(10)
_cell_angle_gamma                63.9550(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7156(2)
_cell_length_b                   15.0052(2)
_cell_length_c                   17.1877(2)
_cell_measurement_reflns_used    34489
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.9620
_cell_measurement_theta_min      4.1690
_cell_volume                     3108.47(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -89.00  33.00   0.50    0.82    --    0.00 -77.00-150.00  244
  2  \w    -27.00  89.00   0.50    0.82    --    0.00  38.00  60.00  232
  3  \w    -27.00  89.00   0.50    0.82    --    0.00  38.00 150.00  232
  4  \w    -27.00  89.00   0.50    0.82    --    0.00  38.00 -30.00  232
  5  \w      1.00 125.00   0.50    0.82    --   36.00  82.00  51.79  248
  6  \w     62.00 177.00   0.50    0.56    --   88.00  45.00 -79.11  230
  7  \w     75.00 195.00   0.50    0.56    --  105.20  30.00 150.00  240
  8  \w     16.00 141.00   0.50    0.56    --  105.20 -82.00  90.00  250
  9  \w     16.00 134.00   0.50    0.56    --  105.20 -61.00 -90.00  236
 10  \w     16.00 141.00   0.50    0.56    --  105.20 -82.00 -30.00  250
 11  \w     75.00 195.00   0.50    0.56    --  105.20  30.00-120.00  240
 12  \w     16.00 134.00   0.50    0.56    --  105.20 -61.00   0.00  236
 13  \w     75.00 195.00   0.50    0.56    --  105.20  30.00-150.00  240
 14  \w     16.00 132.00   0.50    0.56    --  105.20 -82.00 -90.00  232
 15  \w     20.00  45.00   0.50    0.56    --  105.20 -82.00  60.00   50
 16  \w     21.00 141.00   0.50    0.56    --  105.20 -82.00 150.00  240
 17  \w     23.00 133.00   0.50    0.56    --  105.20 -61.00 150.00  220
 18  \w     89.00 114.00   0.50    0.56    --  105.20 -82.00  60.00   50
 19  \w     85.00 174.00   0.50    0.56    --  105.20  45.00 -60.00  178
 20  \w     98.00 124.00   0.50    0.56    --  105.20 -82.00-150.00   52
 21  \w     16.00 138.00   0.50    0.56    --  105.20 -82.00   0.00  244
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115889000
_diffrn_orient_matrix_UB_12      -0.0059717000
_diffrn_orient_matrix_UB_13      0.0877282000
_diffrn_orient_matrix_UB_21      -0.0320318000
_diffrn_orient_matrix_UB_22      -0.0871893000
_diffrn_orient_matrix_UB_23      0.0118982000
_diffrn_orient_matrix_UB_31      0.1228137000
_diffrn_orient_matrix_UB_32      -0.0736525000
_diffrn_orient_matrix_UB_33      -0.0236648000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51920
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.180
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull brownish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.153
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0588P)^2^+5.0187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12338
_reflns_number_total             13118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04019_si_002.cif
_cod_data_source_block           ru_carbene
_cod_original_cell_volume        3108.48(8)
_cod_database_code               4128267
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C64 H60 Br2 Cl2 N5 O4 Ru'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00J(0.025) H00K(0.026) H00L(0.027) H00M(0.024) H00O(0.028)
 H00P(0.026) H00Q(0.03) H00R(0.034) H00S(0.025) H00T(0.024) H00U(0.025)
 H00V(0.035) H00X(0.032) H01D(0.03) H01A(0.047) H01B(0.047) H01C(0.047)
 H01F(0.028) H01G(0.03) H01H(0.031) H01J(0.036) H01K(0.031) H01N(0.038)
 H01Q(0.035) H01E(0.057) H01I(0.057) H01L(0.057) H01M(0.046) H01O(0.046)
 H01V(0.054) H01W(0.044) H01X(0.046) H01Y(0.045) H01Z(0.048) H02C(0.071)
 H011(0.028) H014(0.029) H015(0.03) H016(0.029) H017(0.034) H018(0.035)
 H019(0.03) H020(0.046) H02A(0.064) H02B(0.064) H02D(0.072) H02E(0.072)
 H02F(0.072) H02G(0.069) H02H(0.069) H02I(0.069) H02J(0.073) H02K(0.073)
 H02L(0.073) H026(0.06) H027(0.06) H028(0.067) H02M(0.102) H02N(0.102)
 H02O(0.102)
 Fixed X: H00J(0.605718) H00K(0.59047) H00L(0.89534) H00M(0.714294)
 H00O(0.915911) H00P(0.752259) H00Q(0.724866) H00R(0.976598) H00S(0.769709)
 H00T(0.572488) H00U(0.593366) H00V(1.083639) H00X(0.830919) H01D(0.409311)
 H01A(0.408278) H01B(0.483254) H01C(0.441561) H01F(0.681832) H01G(0.463445)
 H01H(0.277912) H01J(0.484213) H01K(0.498857) H01N(0.71356) H01Q(-0.06459)
 H01E(0.933911) H01I(1.003059) H01L(0.923732) H01M(0.667025) H01O(0.794888)
 H01V(0.60933) H01W(0.290389) H01X(0.191298) H01Y(0.810934) H01Z(0.432885)
 H02C(0.641636) H011(0.483188) H014(0.47682) H016(0.545672) H017(0.034398)
 H018(0.655166) H019(0.309547) H020(0.931626) H02A(0.76083) H02B(0.63209)
 H02D(0.88724) H02E(0.935301) H02F(0.897035) H02G(0.611861) H02H(0.694528)
 H02I(0.567994) H02J(0.50493) H02K(0.480504) H02L(0.527705) H026(0.351374)
 H027(0.723706) H028(0.45548) H02M(0.807717) H02N(0.859406) H02O(0.732413)
 Fixed Y: H00J(0.401067) H00K(0.324282) H00L(0.277658) H00M(0.307105)
 H00O(0.353199) H00P(0.4552) H00Q(0.101037) H00R(0.059066) H00S(0.448522)
 H00T(0.473057) H00U(0.542226) H00V(-0.0932) H00X(-0.051683) H01D(0.523712)
 H01A(0.922656) H01B(0.908995) H01C(1.007037) H01F(0.54509) H01G(0.476771)
 H01H(0.618692) H01J(0.916358) H01K(0.610827) H01N(0.297034) H01Q(0.981634)
 H01E(0.716214) H01I(0.607127) H01L(0.627951) H01M(0.933704) H01O(0.877183)
 H01V(0.673054) H01W(0.924356) H01X(1.053477) H01Y(0.811017) H01Z(0.360561)
 H02C(0.059511) H011(0.738505) H014(0.592216) H016(0.715256) H017(0.854305)
 H018(0.45467) H019(0.730686) H020(0.552125) H02A(0.939843) H02B(0.988209)
 H02D(0.774637) H02E(0.747442) H02F(0.855728) H02G(0.93473) H02H(0.822245)
 H02I(0.853377) H02J(0.805747) H02K(0.811778) H02L(0.880967) H026(0.257131)
 H027(0.160165) H028(0.107097) H02M(0.462159) H02N(0.518344) H02O(0.547373)
 Fixed Z: H00J(0.440869) H00K(0.555101) H00L(0.577079) H00M(0.643486)
 H00O(0.454599) H00P(0.405965) H00Q(0.332469) H00R(0.438229) H00S(0.668196)
 H00T(0.624802) H00U(0.508655) H00V(0.371719) H00X(0.265912) H01D(0.944189)
 H01A(0.724808) H01B(0.640112) H01C(0.689379) H01F(0.766739) H01G(0.805452)
 H01H(0.858189) H01J(0.842988) H01K(0.984374) H01N(0.859396) H01Q(1.13185)
 H01E(0.424557) H01I(0.391398) H01L(0.474779) H01M(0.435247) H01O(0.436188)
 H01V(0.29744) H01W(1.002708) H01X(1.09507) H01Y(0.825137) H01Z(0.89305)
 H02C(0.758275) H011(0.770248) H014(0.721429) H016(0.892179) H017(1.037829)
 H018(0.859532) H019(0.778129) H020(0.302328) H02A(0.557088) H02B(0.559119)
 H02D(0.618446) H02E(0.696681) H02F(0.664457) H02G(0.954231) H02H(0.955172)
 H02I(0.961744) H02J(0.462966) H02K(0.377085) H02L(0.402205) H026(0.879483)
 H027(0.776497) H028(0.81367) H02M(0.252059) H02N(0.18893) H02O(0.202795)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.152
_oxdiff_exptl_absorpt_empirical_full_min 0.505