Controlled Polymerization of Norbornene Cycloparaphenylenes Expands Carbon Nanomaterials Design Space
Maust, Ruth L.; Li, Penghao; Shao, Baihao; Zeitler, Sarah M.; Sun, Peiguan B.; Reid, Harrison W.; Zakharov, Lev N.; Golder, Matthew R.; Jasti, Ramesh; ACS Central Science  (2021) –; doi:10.1021/acscentsci.1c00345

data_4518712
_publ_section_title
;
 Controlled Polymerization of Norbornene Cycloparaphenylenes Expands
 Carbon Nanomaterials Design Space
;
_journal_name_full               'ACS Central Science'
_journal_paper_doi               10.1021/acscentsci.1c00345
_journal_year                    2021
_chemical_formula_sum            'C75 H68'
_chemical_formula_weight         969.29
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.334(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5747(3)
_cell_length_b                   28.3155(16)
_cell_length_c                   32.6239(17)
_cell_measurement_reflns_used    8212
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.54
_cell_measurement_theta_min      2.71
_cell_volume                     6071.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46166
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.698
_diffrn_reflns_theta_max         66.698
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.7025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
Two pentane molecules (C5H12, 42 electrons) highly 
disordered inside the main molecule were tretaed 
by SQUEEZE. 
;
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0732P)^2^+0.5878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8605
_reflns_number_total             10685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc1c00345_si_005.cif
_cod_data_source_block           cu_jasti129_0m_a_sqd
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4518712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.974
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              22410
_shelx_hkl_checksum              75360