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_4027453
_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         'C78 H46 O2'
_chemical_formula_sum            'C78 H46 O2'
_chemical_formula_weight         1015.15
_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                 99.951(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.130(3)
_cell_length_b                   19.101(5)
_cell_length_c                   14.668(4)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.16
_cell_measurement_theta_min      3.70
_cell_volume                     3347.4(15)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.946
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46107
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.77
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
; 
Crystals contain highly disordered mixed solvents (grown from a mixture of 
CH3OH and CH2Cl2) regions which could not be appropriately modelled. 
;
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         9899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1530P)^2^+0.4783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2130
_refine_ls_wR_factor_ref         0.2259
_reflns_number_gt                7758
_reflns_number_total             9899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301223q_si_002.cif
_cod_data_source_block           gg2811-squ
_cod_original_cell_volume        3347.2(15)
_cod_database_code               4027453