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_4027735
_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, C H2 Cl2'
_chemical_formula_sum            'C55 H72 Cl2 O6'
_chemical_formula_weight         900.03
_chemical_name_common            'DR 10 IZOMER II'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6770(3)
_cell_length_b                   14.9810(2)
_cell_length_c                   24.6590(5)
_cell_measurement_reflns_used    26805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     5052.51(17)
_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    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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      -0.691992E-1
_diffrn_orient_matrix_UB_12      0.99717E-2
_diffrn_orient_matrix_UB_13      0.116101E-1
_diffrn_orient_matrix_UB_21      -0.20255E-2
_diffrn_orient_matrix_UB_22      -0.614663E-1
_diffrn_orient_matrix_UB_23      0.157722E-1
_diffrn_orient_matrix_UB_31      0.235242E-1
_diffrn_orient_matrix_UB_32      0.240405E-1
_diffrn_orient_matrix_UB_33      0.355104E-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  0.0409
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29061
_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         26.71
_diffrn_reflns_theta_min         3.1
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.9368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.11(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10372
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+1.4038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2157
_reflns_number_gt                7608
_reflns_number_total             10372
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo3020402_si_002.cif
_cod_data_source_block           san551
_cod_database_code               4027735