Alternating oligo(<i>o</i>,<i>p</i>-phenylenes) <i>via</i> ruthenium catalyzed diol-diene benzannulation: orthogonality to cross-coupling enables <i>de novo</i> nanographene and PAH construction.
Kasun, Zachary A.; Sato, Hiroki; Nie, Jing; Mori, Yasuyuki; Bender, Jon A.; Roberts, Sean T.; Krische, Michael J.; Chemical science 9 (2018) 7866–7873; doi:10.1039/c8sc03236j

data_1549865
_publ_section_title
;
 Alternating oligo(<i>o</i>,<i>p</i>-phenylenes) <i>via</i> ruthenium
 catalyzed diol-diene benzannulation: orthogonality to cross-coupling
 enables <i>de novo</i> nanographene and PAH construction.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              7866
_journal_page_last               7873
_journal_paper_doi               10.1039/c8sc03236j
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C34 H18 S2, 1/3(C H2 Cl2)'
_chemical_formula_sum            'C34.33333 H18.66667 Cl0.66667 S2'
_chemical_formula_weight         518.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-18 deposited with the CCDC.
2018-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.730(11)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   9.2129(16)
_cell_length_b                   21.272(4)
_cell_length_c                   36.423(6)
_cell_measurement_reflns_used    1486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      2.21
_cell_volume                     7135(2)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/Plus, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2014/7, Sheldrick, G. M. 2015'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'Nonius Kappa CCD with Bruker ApexII detector'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1843
_diffrn_reflns_av_unetI/netI     0.1770
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            44139
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        22.873
_diffrn_reflns_theta_max         22.873
_diffrn_reflns_theta_min         1.915
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS. G. M. Sheldrick. Apex II release 2010, Bruker AXS, Inc.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         9603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4755
_reflns_number_total             9603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03236j2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
;

2019-01-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549863--1549865.cif.
;
_cod_original_formula_moiety     '3 C34 H18 S2, C H2 Cl2'
_cod_original_formula_sum        'C103 H56 Cl2 S6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1556.73
_cod_database_code               1549865
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              86903
_shelx_fab_checksum              12570