Axle component separated ion-pair recognition by a neutral heteroditopic [2]rotaxane
Richard C. Knighton; Paul D. Beer; Chem.Commun. 50 (2014) 1540–; doi:10.1039/c3cc48905a

data_7111872
_publ_section_title
;
 Axle component separated ion-pair recognition by a neutral heteroditopic
 [2]rotaxane
;
_journal_coden_Cambridge         182
_journal_name_full               Chem.Commun.
_journal_page_first              1540
_journal_paper_doi               10.1039/c3cc48905a
_journal_volume                  50
_journal_year                    2014
_chemical_compound_source        synthesised
_chemical_formula_moiety         ' C63 H63 N3 O12, C2 H6 O S'
_chemical_formula_sum            'C65 H69 N3 O13 S'
_chemical_formula_weight         1132.34
_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   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                80.423(8)
_cell_angle_beta                 87.747(7)
_cell_angle_gamma                74.632(9)
_cell_formula_units_Z            2
_cell_length_a                   12.6430(12)
_cell_length_b                   14.2835(16)
_cell_length_c                   16.9650(12)
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2912.9(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      0
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.781
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si(1 1 1) double-crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.103
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27664
_diffrn_reflns_theta_full        25.076
_diffrn_reflns_theta_max         29.501
_diffrn_reflns_theta_min         1.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colour
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200.000
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         9464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0979
_refine_ls_shift/su_max          0.0002667
_refine_ls_shift/su_mean         0.0000163
_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: 
 0.724E+04 0.122E+05 0.773E+04 0.331E+04 790. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3130
_refine_ls_wR_factor_gt          0.2492
_refine_ls_wR_factor_ref         0.3129
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6383
_reflns_number_total             13925
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.37
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.1190
_oxford_refine_ls_scale          8.3(5)
_oxford_reflns_number_all        9466
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3cc48905a.txt
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7111872
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  42,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE N   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE N   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   (  53,X'S) H   ( 533,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) H   ( 653,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) H   ( 663,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 672,X'S) H   ( 673,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) H   ( 813,X'S) H   ( 812,X'S) 
RIDE C   (  82,X'S) H   ( 822,X'S) H   ( 821,X'S) H   ( 823,X'S) 
RIDE C   ( 165,X'S) H   (1652,X'S) H   (1651,X'S) H   (1653,X'S) 
RIDE C   ( 166,X'S) H   (1661,X'S) H   (1663,X'S) H   (1662,X'S) 
RIDE C   ( 167,X'S) H   (1673,X'S) H   (1672,X'S) H   (1671,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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