Highly Stereoselective Heterogeneous Diene Polymerization by Co-MFU-4l: A Single-Site Catalyst Prepared by Cation Exchange.
Dubey, Romain J.-C.; Comito, Robert J.; Wu, Zhenwei; Zhang, Guanghui; Rieth, Adam J.; Hendon, Christopher H.; Miller, Jeffrey T.; Dincă, Mircea; Journal of the American Chemical Society 139 (2017) 12664–12669; doi:10.1021/jacs.7b06841

data_4131568
_publ_section_title
;
 Highly Stereoselective Heterogeneous Diene Polymerization by Co-MFU-4l: A
 Single-Site Catalyst Prepared by Cation Exchange.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12664
_journal_page_last               12669
_journal_paper_doi               10.1021/jacs.7b06841
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C39 H45 B Co N6'
_chemical_formula_weight         667.55
_chemical_name_common            'TpMes CoAllyl'
_chemical_name_systematic        'Cobalt Trispyrazolylmesitylborate allyl'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                103.802(3)
_cell_angle_beta                 95.013(3)
_cell_angle_gamma                94.018(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0038(14)
_cell_length_b                   11.3166(17)
_cell_length_c                   17.839(3)
_cell_measurement_reflns_used    23511
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.692
_cell_measurement_theta_min      1.053
_cell_volume                     1750.6(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            112018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.107
_diffrn_reflns_theta_min         1.861
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 7762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         22086
_refine_ls_number_restraints     605
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0645P)^2^+0.1023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.980
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                18468
_reflns_number_total             22086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06841_si_003.cif
_cod_data_source_block           coal
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4131568
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              6841
_shelx_hkl_checksum              13277