A pentagonal cyanostar macrocycle with cyanostilbene CH donors binds anions and forms dialkylphosphate [3]rotaxanes
Semin Lee; Chun-Hsing Chen; Amar H. Flood; Nature Chemistry 5 (2013) 704–710; doi:10.1038/nchem.1668

data_1551391
_publ_section_title
;
 A pentagonal cyanostar macrocycle with cyanostilbene CH donors binds
 anions and forms dialkylphosphate [3]rotaxanes
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              704
_journal_page_last               710
_journal_paper_doi               10.1038/nchem.1668
_journal_volume                  5
_journal_year                    2013
_chemical_absolute_configuration .
_chemical_formula_moiety         'C174.00 H196.00 N17 O13.50 P1'
_chemical_formula_sum            'C174 H196 N17 O13.5 P'
_chemical_formula_weight         2772.55
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                74.262(8)
_cell_angle_beta                 76.314(9)
_cell_angle_gamma                66.192(7)
_cell_formula_units_Z            2
_cell_length_a                   17.781(3)
_cell_length_b                   18.620(3)
_cell_length_c                   31.361(5)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     9048(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28391
_diffrn_reflns_theta_full        23.266
_diffrn_reflns_theta_max         24.235
_diffrn_reflns_theta_min         1.735
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2964.000
_exptl_crystal_size_max          0.947
_exptl_crystal_size_mid          0.776
_exptl_crystal_size_min          0.378
_refine_diff_density_max         1.37
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2320
_refine_ls_number_reflns         28257
_refine_ls_number_restraints     1092
_refine_ls_R_factor_all          0.2004
_refine_ls_R_factor_gt           0.1400
_refine_ls_shift/su_max          0.0497809
_refine_ls_shift/su_mean         0.0023148
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 6.95 8.64 1.96 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3785
_refine_ls_wR_factor_gt          0.3307
_refine_ls_wR_factor_ref         0.3785
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                13256
_reflns_number_total             28391
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.87
_oxford_diffrn_Wilson_scale      292.40
_oxford_refine_ls_r_factor_ref   0.2004
_oxford_refine_ls_scale          0.10907(5)
_oxford_reflns_number_all        28257
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            nchem.1668-s3.cif
_cod_data_source_block           12152
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C174.00 H196.00 N17 O13.50 P1'
_cod_database_code               1551391