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_7107369
_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            'C115.5 H172 Cl21 N12 O20 Zn3'
_chemical_formula_weight         2989.21
_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                 125.19(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.114(11)
_cell_length_b                   18.422(5)
_cell_length_c                   17.181(6)
_cell_measurement_reflns_used    12620
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.79
_cell_volume                     7531(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.938
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27161
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.691
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.5623
_exptl_crystal_size_mid          0.4645
_exptl_crystal_size_min          0.1757
_refine_diff_density_max         1.732
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.053(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.654
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         16403
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.682
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.1002
_refine_ls_shift/su_max          0.013
_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          0.2545
_refine_ls_wR_factor_ref         0.2677
_reflns_number_gt                11124
_reflns_number_total             16403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc16673a.txt
_cod_data_source_block           rthccznb
_cod_original_cell_volume        7531(4)
_cod_original_formula_sum        'C115.50 H172 Cl21 N12 O20 Zn3'
_cod_database_code               7107369