Enantioselective Living Coordinative Chain Transfer Polymerization: Production of Optically Active End-Group-Functionalized (+)- or (−)-Poly(methylene-1,3-cyclopentane) via a Homochiral C1-Symmetric Caproamidinate Hafnium Initiator
Wallace, Mark A.; Zavalij, Peter Y.; Sita, Lawrence R.; ACS Catalysis  (2020) 8496–8502; doi:10.1021/acscatal.0c02104

data_4517861
_publ_section_title
;
 Enantioselective Living Coordinative Chain Transfer Polymerization:
 Production of Optically Active End-Group-Functionalized (+)- or
 (&#x2212;)-Poly(methylene-1,3-cyclopentane) via a Homochiral C1-Symmetric
 Caproamidinate Hafnium Initiator
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              8496
_journal_page_last               8502
_journal_paper_doi               10.1021/acscatal.0c02104
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H40 Hf N2'
_chemical_formula_sum            'C26 H40 Hf N2'
_chemical_formula_weight         559.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4910(4)
_cell_length_b                   9.4910(4)
_cell_length_c                   27.7364(11)
_cell_measurement_reflns_used    25180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.3
_cell_volume                     2498.47(18)
_computing_cell_refinement       'Apex2, Saint (Bruker, 2012)'
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'Olex2 (Dolomanov, 2009)'
_computing_publication_material  'Apex2, SHELXL, Platon (Spek, 2015)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015c)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.1053184
_diffrn_orient_matrix_UB_12      -0.0002188
_diffrn_orient_matrix_UB_13      0.0010312
_diffrn_orient_matrix_UB_21      0.0005813
_diffrn_orient_matrix_UB_22      0.1045929
_diffrn_orient_matrix_UB_23      -0.0043231
_diffrn_orient_matrix_UB_31      -0.0029664
_diffrn_orient_matrix_UB_32      0.0126791
_diffrn_orient_matrix_UB_33      0.0357785
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            44784
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.248
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 3574 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         8106
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0257P)^2^+0.3914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7653
_reflns_number_total             8106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02104_si_003.cif
_cod_data_source_block           cmpd_R_1
_cod_depositor_comments
'Adding full bibliography for 4517861--4517862.cif.'
_cod_original_cell_volume        2498.5(2)
_cod_database_code               4517861
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.299
_shelx_estimated_absorpt_t_max   0.503
_shelx_res_checksum              96660
_shelx_hkl_checksum              69057