Controlling the macrocycle size by the stoichiometry of the applied template ion
Aleksandra Sarnicka; Przemyslaw Starynowicz; Jerzy Lisowski; Chem.Commun. 48 (2012) 2237–; doi:10.1039/c2cc16673a

data_7107368
_publ_section_title
;
 Controlling the macrocycle size by the stoichiometry of the applied
 template ion
;
_journal_name_full               Chem.Commun.
_journal_page_first              2237
_journal_paper_doi               10.1039/c2cc16673a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C116 H192 N12 O25 Zn3'
_chemical_formula_weight         2350.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 113.31(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.17(3)
_cell_length_b                   24.42(2)
_cell_length_c                   18.37(3)
_cell_measurement_reflns_used    8210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.85
_cell_measurement_theta_min      2.81
_cell_volume                     7898(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_device_type  'Kuma KM4 with a CCD counter'
_diffrn_measurement_method       '\w scan'
_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  0.1088
_diffrn_reflns_av_sigmaI/netI    0.3248
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48122
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         36.83
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.5032
_exptl_crystal_size_mid          0.4254
_exptl_crystal_size_min          0.3510
_refine_diff_density_max         3.396
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         26139
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.3311
_refine_ls_R_factor_gt           0.1315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3130
_refine_ls_wR_factor_ref         0.4127
_reflns_number_gt                7720
_reflns_number_total             26139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16673a.txt
_cod_data_source_block           shcczn2
_cod_original_cell_volume        7897(17)
_cod_database_code               7107368