Lanthanide appended rotaxanes respond to changing chloride concentration
Allain, Clémence; Beer, Paul D.; Faulkner, Stephen; Jones, Michael W.; Kenwright, Alan M.; Kilah, Nathan L.; Knighton, Richard C.; Sørensen, Thomas Just; Tropiano, Manuel; Chemical Science 4 (2013) 489–; doi:10.1039/c2sc21614k

data_1514852
_publ_section_title
;
 Lanthanide appended rotaxanes respond to changing chloride concentration
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              489
_journal_paper_doi               10.1039/c2sc21614k
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C70 H102 Lu4 N16 Na4 O31, 12(H2 O)'
_chemical_formula_sum            'C70 H126 Lu4 N16 Na4 O43'
_chemical_formula_weight         2671.69
_chemical_melting_point          ?
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2012-08-29
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 108.6904(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.0616(2)
_cell_length_b                   14.9690(2)
_cell_length_c                   18.2262(3)
_cell_measurement_reflns_used    10960
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4667.84(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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_pressure         105
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            84881
_diffrn_reflns_theta_full        26.949
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.313
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.63
_refine_diff_density_min         -3.05
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10631
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.0067457
_refine_ls_shift/su_mean         0.0000459
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +*****P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1746
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1745
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9306
_reflns_number_total             10639
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.19
_oxford_diffrn_Wilson_scale      70.16
_oxford_refine_ls_r_factor_ref   0.0723
_oxford_refine_ls_scale          0.12582(7)
_oxford_reflns_number_all        10634
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '043mwj11 At 16:48 on 3/ 8'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S
SUMFIX ELEMENT SCALES
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,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 ( 11,X'S) H ( 111,X'S) H ( 112,X'S)
RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S)
RIDE C ( 17,X'S) H ( 172,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S)
RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,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 C ( 38,X'S) H ( 381,X'S) H ( 382,X'S)
RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S)
RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S)
RIDE C ( 46,X'S) H ( 461,X'S)
RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S)
RIDE C ( 49,X'S) H ( 492,X'S) H ( 491,X'S)
RIDE C ( 53,X'S) H ( 531,X'S) H ( 532,X'S)
RIDE O ( 63,X'S) H ( 631,X'S) H ( 632,X'S)
RIDE O ( 66,X'S) H ( 661,X'S) H ( 664,X'S)
RIDE O ( 67,X'S) H ( 671,X'S)
RIDE C ( 1,X'S) H ( 11,X'S)
RIDE O ( 10,X'S) H ( 101,X'S) H ( 103,X'S)
RIDE O ( 680,X'S) H (6801,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S)
RIDE O ( 700,X'S) H (7011,X'S)
RIDE O ( 701,X'S) H (7012,X'S)
RIDE O ( 65,X'S) H ( 652,X'S) H ( 651,X'S)
RIDE O ( 681,X'S) H (6809,X'S)
RIDE O (1501,X'S) H (1505,X'S) H (1502,X'S) H (1503,X'S)
END
;
_iucr_refine_instructions_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = N(37) TO C(38)
U(IJ)'S 0.0, 0.010000 = C(38) TO C(39)
U(IJ)'S 0.0, 0.010000 = C(48) TO C(2)
U(IJ)'S 0.0, 0.010000 = N(34) TO C(48)
U(IJ)'S 0.0, 0.0020000 = C(24) TO C(25)
U(IJ)'S 0.0, 0.0020000 = N(19) TO C(24)
VIBRATION 0.0, 0.020000 = C(24) TO C(25)
VIBRATION 0.0, 0.020000 = N(19) TO C(24)
DISTANCE 1.000000 , 0.200000 = C(36) TO H(361)
DISTANCE 1.000000 , 0.200000 = C(20) TO H(202)
DISTANCE 1.000000 , 0.200000 = C(24) TO H(241)
VIBRATION 0.0, 0.050000 = NA(1) TO O(701)
VIBRATION 0.0, 0.050000 = NA(1) TO O(700)
U(IJ)'S 0.0, 0.050000 = NA(1) TO O(700)
DISTANCE 2.700000 , 0.050000 = NA(1) TO O(700)
DISTANCE 0.850000 , 0.050000 = O(67) TO H(671)
ANGLE 120.000000 , 1.000000 = H(101) TO O(10) TO H(103)
U(IJ)'S 0.0, 0.010000 = O(30) TO C(31)
U(IJ)'S 0.0, 0.010000 = NA(60) TO O(681)
U(IJ)'S 0.0, 0.010000 = NA(60) TO O(680)
DISTANCE 0.90000 , 0.050000 = O(1501) TO H(1502)
DISTANCE 0.90000 , 0.050000 = O(1501) TO H(1505)
ANGLE 120.000000 , 1.000000 = H(1505) TO O(1501) TO H(1502)
DISTANCE 0.850000 , 0.050000 = O(1501) TO H(1503)
END
;
_cod_data_source_file            c2sc21614k.txt
_cod_data_source_block           Lu.5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2yc '
_cod_original_sg_symbol_H-M      'P 2/c '
_cod_database_code               1514852