Crystal Fluidity Reflected by Fast Rotational Motion at the Core, Branches, and Peripheral Aromatic Groups of a Dendrimeric Molecular Rotor.
Jiang, Xing; O'Brien, Zachary J; Yang, Song; Lai, Lan Huong; Buenaflor, Jeffrey; Tan, Colleen; Khan, Saeed; Houk, K. N.; Garcia-Garibay, Miguel A; Journal of the American Chemical Society 138 (2016) 4650–4656; doi:10.1021/jacs.6b01398

data_4130242
_publ_section_title
;
 Crystal Fluidity Reflected by Fast Rotational Motion at the Core,
 Branches, and Peripheral Aromatic Groups of a Dendrimeric Molecular
 Rotor.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4650
_journal_page_last               4656
_journal_paper_doi               10.1021/jacs.6b01398
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C174 H118, 4(C8 H11 N)'
_chemical_formula_sum            'C206 H162 N4'
_chemical_formula_weight         2693.39
_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
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                114.188(2)
_cell_angle_beta                 96.984(3)
_cell_angle_gamma                97.993(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4496(5)
_cell_length_b                   21.0182(10)
_cell_length_c                   23.6119(10)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.43
_cell_measurement_theta_min      2.36
_cell_volume                     4592.2(4)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.945
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92693
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.748
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1426
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; 
  The void electron counts indicates a total of two molecules of C8 H11 N
  were squeezeed from the final refinements. Thus the 
  correct moiety formula should be 'C174 H118, 8(C8 H11 N)'.
  The e- density of the squeezed molecule could not be modeled'
;
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         16066
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0612P)^2^+1.2234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12956
_reflns_number_total             16066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b01398_si_002.cif
_cod_data_source_block           gg1429c-s_sq
_cod_database_code               4130242
_shelxl_version_number           2014/6
_shelx_res_checksum              96132
_shelx_hkl_checksum              9869
_shelx_fab_checksum              17375