Synthesis, crystalline inclusion and structural study of bulkily stoppered and rigid framework molecular constructions
Torsten Müller; Wilhelm Seichter; Edwin Weber; New Journal of Chemistry 30 (2006) 751–; doi:10.1039/b516244k

data_7052239
_publ_section_title
;
 Synthesis, crystalline inclusion and structural study of bulkily
 stoppered and rigid framework molecular constructions
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              751
_journal_paper_doi               10.1039/b516244k
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C57 H62.5 N2.5'
_chemical_formula_weight         782.60
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.037(3)
_cell_angle_beta                 105.183(3)
_cell_angle_gamma                99.764(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7534(6)
_cell_length_b                   11.5581(6)
_cell_length_c                   19.0689(11)
_cell_measurement_temperature    93(2)
_cell_volume                     2211.5(2)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52178
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9544
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       splitter
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                7383
_reflns_number_total             10895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516244k.txt
_cod_data_source_block           tomu_7x_0m
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C57 H62.50 N2.50'
_cod_database_code               7052239