Anisochronous Dynamics in a Crystalline Array of Steroidal Molecular Rotors: Evidence of Correlated Motion within 1D Helical Domains
Braulio Rodríguez-Molina; Norberto Farfán; Margarita Romero; J. Manuel Méndez-Stivalet; Rosa Santillan; Journal of the American Chemical Society 133 (2011) 7280–7283; doi:10.1021/ja2006274

data_4106134
_publ_contact_author_address
;     
      Departamento de Qu\'imica
      Centro de Investigaci\'on y de Estudios Avanzados
      del Instituto Polit\'ecnico Nacional
      Apartado Postal 14-740
      07000 M\'exico, D.F.
      M\'exico
;
_publ_contact_author_email       rsantill@cinvestav.mx
_publ_contact_author_fax         '555 747 3389'
_publ_contact_author_name        'Rosa Santillan'
_publ_contact_author_phone       '555 747 3725'
_publ_section_title
;
 Anisochronous Dynamics in a Crystalline Array of Steroidal Molecular
 Rotors: Evidence of Correlated Motion within 1D Helical Domains
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7280
_journal_page_last               7283
_journal_paper_doi               10.1021/ja2006274
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H54 O4'
_chemical_formula_sum            'C48 H54 O4'
_chemical_formula_weight         694.91
_chemical_name_common            'Compound 2'
_chemical_name_systematic
;
 1,4-bis[3-methoxy-estra-1,3,5-(10)-trien-17\a-ethynyl]phenylene 
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-05-10T17:47:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.873(2)
_cell_length_b                   14.873(2)
_cell_length_c                   14.794(3)
_cell_measurement_reflns_used    10013
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2834.1(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.657533E-1
_diffrn_orient_matrix_UB_12      0.8471E-3
_diffrn_orient_matrix_UB_13      -0.139805E-1
_diffrn_orient_matrix_UB_21      -0.130566E-1
_diffrn_orient_matrix_UB_22      -0.100852E-1
_diffrn_orient_matrix_UB_23      -0.639383E-1
_diffrn_orient_matrix_UB_31      -0.49998E-2
_diffrn_orient_matrix_UB_32      0.374769E-1
_diffrn_orient_matrix_UB_33      -0.01689
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11757
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                2524
_reflns_number_total             3974
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja2006274_si_003.cif
_cod_data_source_block           ucla-p32
_cod_database_code               4106134