Copper(ii)-directed synthesis of neutral heteroditopic [2]rotaxane ion-pair host systems incorporating hydrogen and halogen bonding anion binding cavities
Brown, Asha; Mennie, Katrina M.; Mason, Owen; White, Nicholas G.; Beer, Paul D.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02832F

data_7044345
_publ_section_title
;
 Copper(ii)-directed synthesis of neutral heteroditopic [2]rotaxane
 ion-pair host systems incorporating hydrogen and halogen bonding anion
 binding cavities
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02832F
_journal_year                    2017
_chemical_compound_source        synthesised
_chemical_formula_moiety         'C45 H59  Cu1 I1 N8 O10, 2(Cl O4)'
_chemical_formula_sum            'C45 H59 Cl2 Cu I N8 O18'
_chemical_formula_weight         1261.36
_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
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                72.764(2)
_cell_angle_beta                 89.197(2)
_cell_angle_gamma                68.746(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8265(3)
_cell_length_b                   12.4818(3)
_cell_length_c                   19.5954(5)
_cell_measurement_reflns_used    17507
_cell_measurement_temperature    100
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     2560.57(12)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      100
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36137
_diffrn_reflns_theta_full        25.082
_diffrn_reflns_theta_max         27.263
_diffrn_reflns_theta_min         1.770
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1290
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, di-isopropyl ether'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9513
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9329
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0018934
_refine_ls_shift/su_mean         0.0000377
_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: 
 0.198E+04 0.330E+04 0.205E+04 875. 205. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1080
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1080
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -14
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8502
_reflns_number_total             11094
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.75
_oxford_diffrn_Wilson_scale      0.11
_oxford_refine_ls_r_factor_ref   0.0449
_oxford_refine_ls_scale          3.25(2)
_oxford_reflns_number_all        9329
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7dt02832f2.cif
_cod_data_source_block           pseudorotaxane-3-9-Cu2ClO4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C45 H59 Cl2 Cu1 I1 N8 O18'
_cod_database_code               7044345
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE N   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,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   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE N   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE N   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) 
RIDE O   (  55,X'S) H   ( 551,X'S) 
RIDE N   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) H   ( 593,X'S) H   ( 594,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) H   ( 623,X'S) H   ( 624,X'S) 
RIDE O   (  64,X'S) H   ( 641,X'S) 
RIDE C   ( 160,X'S) H   (1601,X'S) H   (1602,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,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) 
SAME N(58) C(59) C(60) O(61) C(62) C(63) O(64) AND 
CONT N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
DISTANCE 1.52, 0.01 = C(59) TO C(60) C(62) TO C(63) 
DISTANCE 1.42, 0.01 = C(60) TO O(61) O(61) TO C(62) 
CONT C(63) TO O(64) 
DISTANCE 1.52, 0.01 = C(59) TO C(160) 
DISTANCE 1.42, 0.01 = C(160) TO O(161) O(161) TO C(62) 
SIMU 0.02 N(58) C(59) C(60) O(61) C(62) C(63) O(64) 
DELU 0.01 N(58) C(59) C(60) O(61) C(62) C(63) O(64) 
SIMU 0.02 N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
DELU 0.01 N(58) C(59) C(160) O(161) C(62) C(63) O(64) 
REM PERCHLORATE 
DISTANCE 0, 0.01 = MEAN CL(66) TO O(67) CL(66) TO O(68) 
CONT CL(66) TO O(69) CL(66) TO O(70) 
CONT CL(71) TO O(72) CL(71) TO O(73) CL(71) TO O(74) 
CONT CL(71) TO O(75) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.02000 = N(58) TO C(59) 
U(IJ) .0, 0.02000 = C(59) TO C(60) 
U(IJ) .0, 0.02000 = C(59) TO C(160) 
U(IJ) .0, 0.02000 = C(60) TO O(61) 
U(IJ) .0, 0.02000 = O(61) TO C(62) 
U(IJ) .0, 0.02000 = C(62) TO C(63) 
U(IJ) .0, 0.02000 = C(62) TO O(161) 
U(IJ) .0, 0.02000 = C(62) TO C(63) 
U(IJ) .0, 0.04000 = O(64) TO C(63) 
U(IJ) .0, 0.02000 = C(160) TO O(161) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = N(58) TO C(59) 
VIBR .0, 0.00500 = C(59) TO C(56) 
VIBR .0, 0.00200 = C(59) TO C(60) 
VIBR .0, 0.00500 = C(60) TO N(58) 
VIBR .0, 0.00200 = C(59) TO C(160) 
VIBR .0, 0.00500 = C(160) TO N(58) 
VIBR .0, 0.00200 = C(60) TO O(61) 
VIBR .0, 0.00500 = O(61) TO C(59) 
VIBR .0, 0.00200 = O(61) TO C(62) 
VIBR .0, 0.00500 = C(62) TO C(60) 
VIBR .0, 0.00200 = C(62) TO C(63) 
VIBR .0, 0.00500 = C(63) TO O(61) 
VIBR .0, 0.00200 = C(62) TO O(161) 
VIBR .0, 0.00200 = C(62) TO C(63) 
VIBR .0, 0.00500 = C(63) TO O(161) 
VIBR .0, 0.00200 = O(64) TO C(63) 
VIBR .0, 0.00200 = C(160) TO O(161) 
VIBR .0, 0.00500 = O(161) TO C(59) 
VIBR .0, 0.00500 = C(160) TO C(62) 
VIBR .0, 0.00500 = O(64) TO C(62) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;