A calixarene dendron with surface congestion at the first generation.
Galán, Hitos; Murillo, M Teresa; Quesada, Roberto; Escudero-Adán, Eduardo C; Benet-Buchholz, Jordi; Prados, Pilar; de Mendoza, Javier; Chemical communications (Cambridge, England) 46 (2010) 1044–1046; doi:10.1039/b921465h

data_7105242
_publ_section_title
;
 A calixarene dendron with surface congestion at the first generation.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1044
_journal_page_last               1046
_journal_paper_doi               10.1039/b921465h
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C372 H472 N8 O32'
_chemical_formula_weight         5567.58
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.105(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.2509(15)
_cell_length_b                   39.8239(18)
_cell_length_c                   27.5132(12)
_cell_measurement_reflns_used    7027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.13
_cell_measurement_theta_min      2.72
_cell_volume                     37432(3)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 10 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1473
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            248364
_diffrn_reflns_theta_full        23.36
_diffrn_reflns_theta_max         23.36
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Version 2008/1 Bruker-Nonius
Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             12064
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

The structure contains a high number of disordered dimethylsulfoxid molecules

which are difficult to localize. A refined model with disordered solvent

molecules delivered similar R-values as after applying squeeze, but in this

case extremely large thermal displacement parameters were obtained.
Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13

;
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.702
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1931
_refine_ls_number_reflns         27050
_refine_ls_number_restraints     1293
_refine_ls_restrained_S_all      1.757
_refine_ls_R_factor_all          0.2020
_refine_ls_R_factor_gt           0.1364
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3153
_refine_ls_wR_factor_ref         0.3370
_reflns_number_gt                15001
_reflns_number_total             27050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921465h.txt
_cod_data_source_block           hgm215c_0m
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7105242