Macrocyclic Molecular Rotors with Bridged Steroidal Frameworks
Dorota Czajkowska-Szczykowska; Braulio Rodríguez-Molina; Nancy E. Magaña-Vergara; Rosa Santillan; Jacek W. Morzycki; Miguel A. Garcia-Garibay; Journal of Organic Chemistry 77 (2012) 9970–9978; doi:10.1021/jo3020402

data_4027736
_publ_contact_author
;
      Jacek W. Morzycki
      Institute of Chemistry,
      University of Bia\/lystok,
      Pi\/lsudskiego 11/4, 
      15-443 Bia\/lystok, Poland.
;
_publ_contact_author_email       morzycki@uwb.edu.pl
_publ_section_title
;
 Macrocyclic Molecular Rotors with Bridged Steroidal Frameworks
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9970
_journal_page_last               9978
_journal_paper_doi               10.1021/jo3020402
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H70 O6, 1.0(C H2 Cl2)'
_chemical_formula_sum            'C55 H72 Cl2 O6'
_chemical_formula_weight         900.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.0570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8720(4)
_cell_length_b                   6.90200(10)
_cell_length_c                   24.4250(6)
_cell_measurement_reflns_used    25642
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     2543.94(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.967
_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 Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.226823E-1
_diffrn_orient_matrix_UB_12      -0.931635E-1
_diffrn_orient_matrix_UB_13      0.234798E-1
_diffrn_orient_matrix_UB_21      0.220489E-1
_diffrn_orient_matrix_UB_22      0.867724E-1
_diffrn_orient_matrix_UB_23      0.342636E-1
_diffrn_orient_matrix_UB_31      -0.582306E-1
_diffrn_orient_matrix_UB_32      0.691456E-1
_diffrn_orient_matrix_UB_33      -0.113627E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25703
_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        25.5
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.126
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         10396
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                6403
_reflns_number_total             10396
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo3020402_si_003.cif
_cod_data_source_block           san567
_cod_database_code               4027736