Calix[4]phyrins. Effect of Peripheral Substituents on Conformational Mobility and Structure within a Series of Related Systems
Bohumil Dolenský; Jiří Kroulík; Vladimír Král; Jonathan L. Sessler; Hana Dvořáková; Petr Bouř; Markéta Bernátková; Christophe Bucher; Vincent Lynch; Journal of the American Chemical Society 126 (2004) 13714–13722; doi:10.1021/ja048075g

data_4113096
_publ_section_title
;
 Calix[4]phyrins. Effect of Peripheral Substituents on Conformational
 Mobility and Structure within a Series of Related Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13714
_journal_page_last               13722
_journal_paper_doi               10.1021/ja048075g
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C57 H27 Cl3 F10 N4'
_chemical_formula_weight         1064.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 107.054(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0933(2)
_cell_length_b                   24.4686(3)
_cell_length_c                   13.2314(2)
_cell_measurement_temperature    153(2)
_cell_volume                     4671.65(11)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;
SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10374
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.56(8)
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         10360
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+3.6146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                7645
_reflns_number_total             10360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048075gsi20040403_012411.cif
_cod_data_source_block           1c
_cod_database_code               4113096