Solid-State Molecular Rotors with Perdeuterated Stators: Mechanistic Insights from Biphenylene Rotational Dynamics in Ordered and Disordered Crystal Forms
Zachary J. O'Brien; Steven D. Karlen; Saeed Khan; Miguel A. Garcia-Garibay; Journal of Organic Chemistry 75 (2010) 2482–2491; doi:10.1021/jo9025176

data_4025377
_publ_section_title
;
 Solid-State Molecular Rotors with Perdeuterated Stators: Mechanistic
 Insights from Biphenylene Rotational Dynamics in Ordered and Disordered
 Crystal Forms
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2482
_journal_page_last               2491
_journal_paper_doi               10.1021/jo9025176
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C56 H38'
_chemical_formula_sum            'C56 H38'
_chemical_formula_weight         710.86
_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                 102.739(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5969(12)
_cell_length_b                   14.440(2)
_cell_length_c                   16.362(2)
_cell_measurement_reflns_used    1393
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.27
_cell_measurement_theta_min      2.48
_cell_volume                     1981.2(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1103
_diffrn_reflns_av_sigmaI/netI    0.1489
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17689
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9988
_exptl_absorpt_correction_T_min  0.9356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.125
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.2240
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                1680
_reflns_number_total             4812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9025176_si_002.cif
_cod_data_source_block           gg1005sm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1981.1(5)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4025377