Toward Crystalline Molecular Rotors with Linearly Conjugated Diethynyl-Phenylene Rotators and Pentiptycene Stators
Edgar Escalante-Sánchez; Braulio Rodríguez-Molina; Miguel A. Garcia-Garibay; Journal of Organic Chemistry 77 (2012) 7428–7434; doi:10.1021/jo301223q

data_4027454
_publ_contact_author_address
;     
      Chemistry and Biochemistry Department
      University of California Los Angeles
      Charles E. Young Drive East
      Los Angeles, CA 90095
      USA
;
_publ_contact_author_email       mgg@chem.ucla.edu
_publ_contact_author_fax         '310 825 3159'
_publ_contact_author_name        'Miguel A. Garcia-Garibay'
_publ_contact_author_phone       '310 825 3159'
_publ_section_title
;
 Toward Crystalline Molecular Rotors with Linearly Conjugated
 Diethynyl-Phenylene Rotators and Pentiptycene Stators
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7428
_journal_page_last               7434
_journal_paper_doi               10.1021/jo301223q
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C82 H50 O4'
_chemical_formula_sum            'C82 H50 O4'
_chemical_formula_weight         1099.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5315(10)
_cell_length_b                   21.487(2)
_cell_length_c                   17.0652(19)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      3.64
_cell_volume                     3418.6(6)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45719
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9961
_exptl_absorpt_correction_T_min  0.9715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The solvent sites in lattice could not be modelled and thus their
contribution were squeezed from final refinements. The sites are 
likely a mixture of CH2Cl2, CHCl3 and hexanes. 
;
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         9213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+0.2577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2099
_reflns_number_gt                6915
_reflns_number_total             9213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301223q_si_003.cif
_cod_data_source_block           gg2011s
_cod_original_cell_volume        3418.7(6)
_cod_database_code               4027454