Synthesis of Highly Cis, Syndiotactic Polymers via Ring-Opening Metathesis Polymerization Using Ruthenium Metathesis Catalysts
Lauren E. Rosebrugh; Vanessa M. Marx; Benjamin K. Keitz; Robert H. Grubbs; Journal of the American Chemical Society 135 (2013) 10032–10035; doi:10.1021/ja405559y

data_4120088
_publ_contact_author_address
;
Beckman Institute
Caltech 139-74
Pasadena CA 91125
USA
;
_publ_contact_author_email       xray@caltech.edu
_publ_contact_author_name        'Xray Staff'
_publ_section_title
;
 Synthesis of Highly Cis, Syndiotactic Polymers via Ring-Opening
 Metathesis Polymerization Using Ruthenium Metathesis Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10032
_journal_page_last               10035
_journal_paper_doi               10.1021/ja405559y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C32 H46 N2 O3 Ru'
_chemical_formula_sum            'C32 H46 N2 O3 Ru'
_chemical_formula_weight         607.78
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
 SHELXL-2013 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 103.793(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0782(5)
_cell_length_b                   27.9893(11)
_cell_length_c                   10.2073(4)
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.77
_cell_measurement_theta_min      2.39
_cell_volume                     3073.7(2)
_computing_cell_refinement       'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2012.10-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
 and SHELXL.
;
_computing_structure_refinement  'SHELXL-2013/2 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            191072
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         39.114
_diffrn_reflns_theta_min         2.028
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0634 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.9194.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.792
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         17585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.468
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_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^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13528
_reflns_number_total             17585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja405559y_si_002.cif
_cod_data_source_block           vmm03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4120088
_exptl_crystal_colour_actual     'dichroic, dark purple and light blue'
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.943
_shelxl_version_number           2013-2
_shelx_res_checksum              70575