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_4517862
_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           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_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                   9.4877(6)
_cell_length_b                   9.4877(6)
_cell_length_c                   27.766(2)
_cell_measurement_reflns_used    17405
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.3
_cell_volume                     2499.4(3)
_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      0.0245418
_diffrn_orient_matrix_UB_12      0.0904113
_diffrn_orient_matrix_UB_13      0.0165085
_diffrn_orient_matrix_UB_21      -0.0942680
_diffrn_orient_matrix_UB_22      0.0004129
_diffrn_orient_matrix_UB_23      0.0160949
_diffrn_orient_matrix_UB_31      0.0401838
_diffrn_orient_matrix_UB_32      -0.0542212
_diffrn_orient_matrix_UB_33      0.0276674
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0201
_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            33785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.248
_diffrn_reflns_theta_min         2.147
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.187
_exptl_absorpt_correction_T_max  0.415
_exptl_absorpt_correction_T_min  0.307
_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          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 3515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(4)
_refine_ls_extinction_coef       0.00041(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         8065
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0165
_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^)+(0.0204P)^2^+0.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0378
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                7523
_reflns_number_total             8065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02104_si_002.cif
_cod_data_source_block           cmpd_S_1
_cod_depositor_comments
'Adding full bibliography for 4517861--4517862.cif.'
_cod_original_cell_volume        2499.4(4)
_cod_database_code               4517862
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.322
_shelx_estimated_absorpt_t_max   0.473
_shelx_res_checksum              81225
_shelx_hkl_checksum              23049