Crystalline Arrays of Pairs of Molecular Rotors: Correlated Motion, Rotational Barriers, and Space-Inversion Symmetry Breaking Due to Conformational Mutations
Cyprien Lemouchi; Konstantinos Iliopoulos; Leokadiya Zorina; Sergey Simonov; Pawel Wzietek; Thomas Cauchy; Antonio Rodríguez-Fortea; Enric Canadell; Jiří Kaleta; Josef Michl; Denis Gindre; Michael Chrysos; Patrick Batail; Journal of the American Chemical Society 135 (2013) 9366–9376; doi:10.1021/ja4044517

data_4119996
_publ_contact_author_address
;
Laboratoire MOLTECH-Anjou, CNRS, Universit\'e d'Angers,
UMR 6200, 49045 Angers, France
;
_publ_contact_author_email       patrick.batail@univ-angers.fr
_publ_contact_author_name        'Dr. Patrick Batail'
_publ_section_title
;
 Crystalline Arrays of Pairs of Molecular Rotors: Correlated Motion,
 Rotational Barriers, and Space-Inversion Symmetry Breaking Due to
 Conformational Mutations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9366
_journal_page_last               9376
_journal_paper_doi               10.1021/ja4044517
_journal_volume                  135
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H32 N2'
_chemical_formula_sum            'C34 H32 N2'
_chemical_formula_weight         468.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.300(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.3333(16)
_cell_length_b                   8.3151(5)
_cell_length_c                   10.2204(9)
_cell_measurement_temperature    200(1)
_cell_volume                     2646.7(3)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       'combined \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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20793
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0805P)^2^+4.2370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                1844
_reflns_number_total             3152
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja4044517_si_003.cif
_cod_data_source_block           doubleBCO,200K
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4119996