Polymorphism or pseudopolymorphism of a macrocyclic compound: helical structure, layered structure and pseudorotaxane constructed by weak intermolecular interactions
Tohaya, Taichi; Katagiri, Kosuke; Katoh, Junya; Masu, Hyuma; Tominaga, Masahide; Azumaya, Isao; CrystEngComm 12 (2010) 3493–; doi:10.1039/c0ce00058b

data_7212773
_publ_section_title
;
 Polymorphism or pseudopolymorphism of a macrocyclic compound: helical
 structure, layered structure and pseudorotaxane constructed by weak
 intermolecular interactions
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3493
_journal_paper_doi               10.1039/c0ce00058b
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C48 H42'
_chemical_formula_weight         618.82
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.4000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9511(13)
_cell_length_b                   24.458(3)
_cell_length_c                   13.2818(14)
_cell_measurement_reflns_used    3536
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.36
_cell_volume                     3563.0(7)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16772
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+1.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1742
_reflns_number_gt                3985
_reflns_number_total             7073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00058b.txt
_cod_data_source_block           compound1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3562.9(7)
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7212773