Breaking the Bimolecular Crystal: The Effect of Side-Chain Length on Oligothiophene/Fullerene Intercalation
Burnett, Edmund K.; Cherniawski, Benjamin P.; Rosa, Stephen J.; Smilgies, Detlef-M.; Parkin, Sean; Briseno, Alejandro L.; Chemistry of Materials 30 (2018) 2550–; doi:10.1021/acs.chemmater.7b04702

data_4003110
_publ_section_title
;
 Breaking the Bimolecular Crystal: The Effect of Side-Chain Length on
 Oligothiophene/Fullerene Intercalation
;
_journal_issue                   8
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2550
_journal_paper_doi               10.1021/acs.chemmater.7b04702
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'C68 H94 S8'
_chemical_formula_sum            'C68 H94 S8'
_chemical_formula_weight         1167.91
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.753(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8513(3)
_cell_length_b                   34.8811(10)
_cell_length_c                   37.7740(11)
_cell_measurement_reflns_used    9175
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      74.71
_cell_measurement_theta_min      2.79
_cell_volume                     12978.9(7)
_computing_cell_refinement       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_reduction        '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2016/6</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            105127
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.900
_diffrn_reflns_theta_min         2.533
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause et al., 2015)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       lath
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
; 
Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         22523
_refine_ls_number_restraints     2155
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+45.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                14930
_reflns_number_total             22523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04702_si_002.cif
_cod_data_source_block           c17013
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4003110
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.397
_shelx_estimated_absorpt_t_max   0.972
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;
_shelx_res_checksum              11933
_shelx_hkl_checksum              86377