‘Sacrificial’ Supramolecular Assembly and Pressure-Induced Polymerization: Toward Sequence-Defined Functionalized Nanothreads
Gerthoffer, Margaret C.; Wu, Sikai; Chen, Bo; Wang, Tao; Huss, Steven; Oburn, Shalisa M.; Crespi, Vincent; Badding, John; Elacqua, Elizabeth; Chemical Science  (2020) –; doi:10.1039/D0SC03904G

data_1558974
_publ_section_title
;
 &#x2018;Sacrificial&#x2019; Supramolecular Assembly and Pressure-Induced
 Polymerization: Toward Sequence-Defined Functionalized Nanothreads
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03904G
_journal_year                    2020
_chemical_formula_moiety         'C6 H F5 O, C6 H6 O'
_chemical_formula_sum            'C12 H7 F5 O2'
_chemical_formula_weight         278.18
_chemical_name_systematic        'Phenol Pentafluorophenol'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-12 deposited with the CCDC.	2020-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   7.4348(6)
_cell_length_b                   23.1324(18)
_cell_length_c                   20.2671(16)
_cell_measurement_reflns_used    4629
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.177
_cell_measurement_theta_min      2.672
_cell_volume                     3485.6(5)
_computing_cell_refinement       'SAINT V6.36A (BRUKER, 2001)'
_computing_data_collection       'SMART V5.634 (Bruker Inc., 2009)'
_computing_data_reduction        'SAINT V6.36A (BRUKER, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12695
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.345906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.05 (BRUKER, 2001) was used for absorption correction.
R(int) was 0.0631 before and 0.0331 after correction.
The Ratio of minimum to maximum transmission is 0.3459.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexanes'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.116
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details
;
 Flack x determined using 1972 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.8(3)
_refine_ls_extinction_coef       0.0070(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         6051
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.0105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                4844
_reflns_number_total             6051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03904g2.cif
_cod_data_source_block           eze1s
_cod_depositor_comments
;

2022-03-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '3(C6 H F5 O), 3(C6 H6 O)'
_cod_original_formula_sum        'C36 H21 F15 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     834.53
_cod_database_code               1558974
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O4(H4), O2(H2), O5(H5), O6(H6)
;
_shelx_res_checksum              9242
_olex2_submission_special_instructions 'No special instructions were received'