Atomically precise organomimetic cluster nanomolecules assembled via perfluoroaryl-thiol SNAr chemistry
Elaine A. Qian; Alex I. Wixtrom; Jonathan C. Axtell; Azin Saebi; Dahee Jung; Pavel Rehak; Yanxiao Han; Elamar Hakim Moully; Daniel Mosallaei; Sylvia Chow; Marco S. Messina; Jing Yang Wang; A. Timothy Royappa; Arnold L. Rheingold; Heather D. Maynard; Petr Kral; Alexander M. Spokoyny; Nature Chemistry 9 (2017) 333–340; doi:10.1038/nchem.2686

data_1551833
_publ_section_title
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 Atomically precise organomimetic cluster nanomolecules assembled via
 perfluoroaryl-thiol SNAr chemistry
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              333
_journal_page_last               340
_journal_paper_doi               10.1038/nchem.2686
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         '2(C78 H36 B6 F30 O6)'
_chemical_formula_sum            'C156 H72 B12 F60 O12'
_chemical_formula_weight         3407.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                97.606(5)
_cell_angle_beta                 114.089(5)
_cell_angle_gamma                109.756(5)
_cell_formula_units_Z            2
_cell_length_a                   19.211(3)
_cell_length_b                   19.674(3)
_cell_length_c                   22.866(4)
_cell_measurement_reflns_used    8797
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.817
_cell_measurement_theta_min      2.323
_cell_volume                     7048(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.1157
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            111260
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.381
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         1.196
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8965.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2161
_refine_ls_number_reflns         25783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0831P)^2^+5.5490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11893
_reflns_number_total             25783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nchem.2686-s3.cif
_cod_data_source_block           spok22_a
_cod_original_cell_volume        7047.9(18)
_cod_database_code               1551833
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.036) H1B(0.036) H3(0.084) H069(0.086) H5(0.081) H6(0.079)
 H13C(0.031) H13D(0.031) H15(0.032) H16(0.035) H18(0.044) H19(0.041)
 H26A(0.043) H26B(0.043) H28(0.042) H29(0.039) H31(0.042) H32(0.042)
 H39A(0.028) H39B(0.028) H41(0.029) H42(0.031) H44(0.034) H45(0.034)
 H52A(0.033) H52B(0.033) H54(0.037) H55(0.04) H57(0.043) H58(0.039) H65A(0.032)
 H65B(0.032) H67(0.037) H68(0.041) H70(0.051) H71(0.041) H72A(0.031)
 H72B(0.031) H74(0.047) H75(0.061) H77(0.057) H78(0.043) H85A(0.03) H85B(0.03)
 H87(0.049) H88(0.058) H90(0.049) H91(0.041) H98A(0.028) H98B(0.028)
 H104(0.031) H103(0.036) H101(0.042) H100(0.036) H11A(0.03) H11B(0.03)
 H113(0.037) H114(0.04) H116(0.053) H117(0.043) H12A(0.028) H12B(0.028)
 H130(0.032) H129(0.037) H127(0.052) H126(0.046) H13A(0.034) H13B(0.034)
 H143(0.034) H142(0.037) H140(0.047) H139(0.044)
 Fixed X: H1A(0.6698) H1B(0.727) H3(0.7067) H069(0.8116) H5(0.9519) H6(0.8485)
 H13C(0.5831) H13D(0.6664) H15(0.5909) H16(0.6648) H18(0.8814) H19(0.8077)
 H26A(0.6083) H26B(0.5115) H28(0.6332) H29(0.5886) H31(0.3608) H32(0.4061)
 H39A(0.4394) H39B(0.3789) H41(0.3267) H42(0.2136) H44(0.1961) H45(0.3083)
 H52A(0.2575) H52B(0.2624) H54(0.2215) H55(0.095) H57(-0.0209) H58(0.1068)
 H65A(0.4138) H65B(0.405) H67(0.4469) H68(0.5134) H70(0.6073) H71(0.5437)
 H72A(0.618) H72B(0.5644) H74(0.7109) H75(0.8316) H77(0.7896) H78(0.6694)
 H85A(0.6818) H85B(0.7384) H87(0.8751) H88(0.9711) H90(0.7804) H91(0.6855)
 H98A(0.582) H98B(0.6635) H104(0.5927) H103(0.6689) H101(0.8849) H100(0.8083)
 H11A(0.4217) H11B(0.4109) H113(0.447) H114(0.5194) H116(0.6351) H117(0.5658)
 H12A(0.2743) H12B(0.2635) H130(0.1279) H129(-0.0025) H127(0.082) H126(0.2118)
 H13A(0.4873) H13B(0.3911) H143(0.5843) H142(0.6312) H140(0.428) H139(0.3811)
 Fixed Y: H1A(0.7302) H1B(0.6912) H3(0.7961) H069(0.8601) H5(0.7635) H6(0.7)
 H13C(0.66) H13D(0.665) H15(0.7778) H16(0.9013) H18(0.8761) H19(0.7542)
 H26A(0.4903) H26B(0.4742) H28(0.3673) H29(0.25) H31(0.2476) H32(0.3653)
 H39A(0.6332) H39B(0.5883) H41(0.4367) H42(0.3776) H44(0.5757) H45(0.6352)
 H52A(0.5172) H52B(0.4371) H54(0.51) H55(0.4597) H57(0.3224) H58(0.37)
 H65A(0.6497) H65B(0.6799) H67(0.8123) H68(0.9366) H70(0.8678) H71(0.7435)
 H72A(0.4139) H72B(0.3787) H74(0.3843) H75(0.4497) H77(0.637) H78(0.5722)
 H85A(0.7297) H85B(0.686) H87(0.7453) H88(0.8128) H90(0.8176) H91(0.7512)
 H98A(0.6505) H98B(0.6519) H104(0.7701) H103(0.8934) H101(0.8671) H100(0.7453)
 H11A(0.6552) H11B(0.6843) H113(0.814) H114(0.9405) H116(0.8748) H117(0.7503)
 H12A(0.5384) H12B(0.4524) H130(0.5176) H129(0.4729) H127(0.3765) H126(0.4198)
 H13A(0.5322) H13B(0.5199) H143(0.6309) H142(0.7488) H140(0.7714) H139(0.6542)
 Fixed Z: H1A(0.6246) H1B(0.615) H3(0.7405) H069(0.8521) H5(0.8239) H6(0.7123)
 H13C(0.4255) H13D(0.4222) H15(0.4742) H16(0.5487) H18(0.6145) H19(0.5375)
 H26A(0.3506) H26B(0.3262) H28(0.3405) H29(0.2659) H31(0.156) H32(0.2314)
 H39A(0.3468) H39B(0.3741) H41(0.2631) H42(0.1532) H44(0.1481) H45(0.2584)
 H52A(0.4761) H52B(0.4636) H54(0.3274) H55(0.2256) H57(0.3066) H58(0.4066)
 H65A(0.5318) H65B(0.4684) H67(0.4866) H68(0.5572) H70(0.7183) H71(0.6473)
 H72A(0.1289) H72B(0.1646) H74(0.2392) H75(0.3436) H77(0.3485) H78(0.2413)
 H85A(0.1166) H85B(0.1149) H87(0.2069) H88(0.3209) H90(0.3522) H91(0.2395)
 H98A(-0.082) H98B(-0.0867) H104(-0.0328) H103(0.0411) H101(0.0974)
 H100(0.0212) H11A(0.0311) H11B(-0.0331) H113(-0.0149) H114(0.055) H116(0.2129)
 H117(0.1426) H12A(-0.0162) H12B(-0.0318) H130(-0.0702) H129(-0.1665) H127(-
 0.2735) H126(-0.1761) H13A(0.1734) H13B(0.1466) H143(0.2771) H142(0.3527)
 H140(0.2249) H139(0.1498)
;
_shelx_res_checksum              37417
_shelx_hkl_checksum              61789