Synthesis, Structure, and Complexation of a Large 28-mer Macrocycle Containing Two Binding Sites for Either Anions or Metal Ions
Leroy Cronin; Pamela A. McGregor; Simon Parsons; Simon Teat; Robert O. Gould; Vivienne A. White; Nicholas J. Long; Neil Robertson; Inorganic Chemistry 43 (2004) 8023–8029; doi:10.1021/ic049190v

data_4312173
_publ_section_title
;
 Synthesis, Structure, and Complexation of a Large 28-mer Macrocycle
 Containing Two Binding Sites for Either Anions or Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8023
_journal_page_last               8029
_journal_paper_doi               10.1021/ic049190v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C20 H52 N12 O20'
_chemical_formula_weight         780.74
_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   'geometric/difference map (H2O)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.86(5)
_cell_angle_beta                 83.68(5)
_cell_angle_gamma                64.05(4)
_cell_formula_units_Z            2
_cell_length_a                   11.596(3)
_cell_length_b                   11.803(6)
_cell_length_c                   14.575(7)
_cell_measurement_temperature    150(2)
_cell_volume                     1780.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Bruker Smart, st. 9.8, Daresbury'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68840
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.1814
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12280
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.045(7)
_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   1.062
_refine_ls_hydrogen_treatment    'Riding/rotating group (H2O)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9063
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1996
_refine_ls_R_factor_gt           0.1197
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1725P)^2^+6.6895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3440
_refine_ls_wR_factor_ref         0.3664
_reflns_number_gt                4787
_reflns_number_total             9063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049190vsi20040621_110700_2.cif
_cod_data_source_block           pm110a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        1780.5(13)
_cod_database_code               4312173