Polyyne Rotaxanes: Stabilization by Encapsulation.
Movsisyan, Levon D.; Franz, Michael; Hampel, Frank; Thompson, Amber L.; Tykwinski, Rik R.; Anderson, Harry L.; Journal of the American Chemical Society 138 (2016) 1366–1376; doi:10.1021/jacs.5b12049

data_4129941
_publ_section_title
;
 Polyyne Rotaxanes: Stabilization by Encapsulation.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1366
_journal_page_last               1376
_journal_paper_doi               10.1021/jacs.5b12049
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C102 H126, C42 H42 N2 O4'
_chemical_formula_sum            'C144 H168 N2 O4'
_chemical_formula_weight         1990.93
_chemical_melting_point          ?
_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_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-09-16
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                98.118(3)
_cell_angle_beta                 97.637(3)
_cell_angle_gamma                90.506(3)
_cell_formula_units_Z            2
_cell_length_a                   14.5311(5)
_cell_length_b                   15.0614(5)
_cell_length_c                   28.4507(9)
_cell_measurement_reflns_used    20252
_cell_measurement_temperature    100
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     6107.2(4)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_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      100
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.859
_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  0.042
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            95494
_diffrn_reflns_theta_full        24.400
_diffrn_reflns_theta_max         28.465
_diffrn_reflns_theta_min         1.588
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.40
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9303
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         25074
_refine_ls_number_restraints     508
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.0005124
_refine_ls_shift/su_mean         0.0000403
_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: 
 0.183E+04 0.284E+04 0.148E+04 385. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1647
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1647
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                19718
_reflns_number_total             29087
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0885
_oxford_refine_ls_scale          3.70(2)
_oxford_reflns_number_all        25074
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0202
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S 
CONT C(1,U'S) UNTIL C(254) 
EQUIV C(262,U[ISO]) UNTIL C(267) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
WEIGHT -1 PART(3002,OCC) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) H   ( 493,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) H   ( 503,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   ( 531,X'S) H   ( 532,X'S) H   ( 533,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) H   ( 543,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 682,X'S) H   ( 683,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 692,X'S) H   ( 693,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 702,X'S) H   ( 703,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) H   ( 723,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) H   ( 733,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) H   ( 743,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) H   ( 882,X'S) H   ( 883,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) H   ( 892,X'S) H   ( 893,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) H   ( 902,X'S) H   ( 903,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) H   ( 922,X'S) H   ( 923,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) H   ( 932,X'S) H   ( 933,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) H   ( 942,X'S) H   ( 943,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1082,X'S) H   (1083,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1092,X'S) H   (1093,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1102,X'S) H   (1103,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) H   (1123,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) H   (1133,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) H   (1142,X'S) H   (1143,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) H   (1282,X'S) H   (1283,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) H   (1292,X'S) H   (1293,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) H   (1302,X'S) H   (1303,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) H   (1322,X'S) H   (1323,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) H   (1332,X'S) H   (1333,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) H   (1342,X'S) H   (1343,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) 
RIDE C   ( 147,X'S) H   (1471,X'S) 
RIDE C   ( 148,X'S) H   (1481,X'S) 
RIDE C   ( 150,X'S) H   (1501,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) 
RIDE C   ( 156,X'S) H   (1561,X'S) 
RIDE C   ( 157,X'S) H   (1571,X'S) 
RIDE C   ( 159,X'S) H   (1591,X'S) 
RIDE C   ( 160,X'S) H   (1601,X'S) 
RIDE C   ( 162,X'S) H   (1621,X'S) H   (1622,X'S) 
RIDE C   ( 163,X'S) H   (1631,X'S) H   (1632,X'S) 
RIDE C   ( 164,X'S) H   (1641,X'S) H   (1642,X'S) 
RIDE C   ( 165,X'S) H   (1651,X'S) H   (1652,X'S) 
RIDE C   ( 166,X'S) H   (1661,X'S) H   (1662,X'S) 
CONT C   ( 266,X'S) H   (2661,X'S) H   (2662,X'S) 
RIDE C   ( 167,X'S) H   (1671,X'S) H   (1672,X'S) 
RIDE C   ( 170,X'S) H   (1701,X'S) 
RIDE C   ( 171,X'S) H   (1711,X'S) 
RIDE C   ( 173,X'S) H   (1731,X'S) 
RIDE C   ( 174,X'S) H   (1741,X'S) 
RIDE C   ( 176,X'S) H   (1761,X'S) H   (1762,X'S) 
RIDE C   ( 177,X'S) H   (1771,X'S) H   (1772,X'S) 
RIDE C   ( 178,X'S) H   (1781,X'S) H   (1782,X'S) 
RIDE C   ( 179,X'S) H   (1791,X'S) H   (1792,X'S) 
RIDE C   ( 180,X'S) H   (1801,X'S) H   (1802,X'S) 
RIDE C   ( 181,X'S) H   (1811,X'S) H   (1812,X'S) 
RIDE C   ( 183,X'S) H   (1831,X'S) 
RIDE C   ( 185,X'S) H   (1851,X'S) 
RIDE C   ( 186,X'S) H   (1861,X'S) 
RIDE C   ( 187,X'S) H   (1871,X'S) 
RIDE C   ( 212,X'S) H   (2121,X'S) H   (2122,X'S) H   (2123,X'S) 
RIDE C   ( 213,X'S) H   (2131,X'S) H   (2132,X'S) H   (2133,X'S) 
RIDE C   ( 214,X'S) H   (2141,X'S) H   (2142,X'S) H   (2143,X'S) 
RIDE C   ( 252,X'S) H   (2521,X'S) H   (2522,X'S) H   (2523,X'S) 
RIDE C   ( 253,X'S) H   (2531,X'S) H   (2532,X'S) H   (2533,X'S) 
RIDE C   ( 254,X'S) H   (2541,X'S) H   (2542,X'S) H   (2543,X'S) 
RIDE C   ( 262,X'S) H   (2621,X'S) H   (2622,X'S) 
RIDE C   ( 263,X'S) H   (2631,X'S) H   (2632,X'S) 
RIDE C   ( 264,X'S) H   (2641,X'S) H   (2642,X'S) 
RIDE C   ( 265,X'S) H   (2651,X'S) H   (2652,X'S) 
RIDE C   ( 267,X'S) H   (2671,X'S) H   (2672,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SAME  C(45)  C(51)  C(52)  C(53)  C(54)  AND 
CONT  C(45)  C(51)  C(53)  C(54)  C(52)  AND 
CONT  C(45)  C(51)  C(54)  C(52)  C(53)  AND 
CONT  C(45)  C(51)  C(252)  C(253)  C(254)  AND 
CONT  C(45)  C(51)  C(253)  C(254)  C(252)  AND 
CONT  C(45)  C(51)  C(254)  C(252)  C(253) 
SAME  C(105)  C(111)  C(112)  C(113)  C(114)  AND 
CONT  C(105)  C(111)  C(113)  C(114)  C(112)  AND 
CONT  C(105)  C(111)  C(114)  C(112)  C(113)  AND 
CONT  C(105)  C(111)  C(212)  C(213)  C(214)  AND 
CONT  C(105)  C(111)  C(213)  C(214)  C(212)  AND 
CONT  C(105)  C(111)  C(214)  C(212)  C(213) 
SIMU  0.01  C(45)  C(51)  C(52)  C(53)  C(54)  AND 
CONT  C(45)  C(51)  C(53)  C(54)  C(52)  AND 
CONT  C(45)  C(51)  C(54)  C(52)  C(53)  AND 
CONT  C(45)  C(51)  C(252)  C(253)  C(254)  AND 
CONT  C(45)  C(51)  C(253)  C(254)  C(252)  AND 
CONT  C(45)  C(51)  C(254)  C(252)  C(253) 
SIMU  0.01  C(105)  C(111)  C(112)  C(113)  C(114)  AND 
CONT  C(105)  C(111)  C(113)  C(114)  C(112)  AND 
CONT  C(105)  C(111)  C(114)  C(112)  C(113)  AND 
CONT  C(105)  C(111)  C(212)  C(213)  C(214)  AND 
CONT  C(105)  C(111)  C(213)  C(214)  C(212)  AND 
CONT  C(105)  C(111)  C(214)  C(212)  C(213) 
DELU  0.01  C(45)  C(51)  C(52)  C(53)  C(54)  AND 
CONT  C(45)  C(51)  C(53)  C(54)  C(52)  AND 
CONT  C(45)  C(51)  C(54)  C(52)  C(53)  AND 
CONT  C(45)  C(51)  C(252)  C(253)  C(254)  AND 
CONT  C(45)  C(51)  C(253)  C(254)  C(252)  AND 
CONT  C(45)  C(51)  C(254)  C(252)  C(253) 
DELU  0.01  C(105)  C(111)  C(112)  C(113)  C(114)  AND 
CONT  C(105)  C(111)  C(113)  C(114)  C(112)  AND 
CONT  C(105)  C(111)  C(114)  C(112)  C(113)  AND 
CONT  C(105)  C(111)  C(212)  C(213)  C(214)  AND 
CONT  C(105)  C(111)  C(213)  C(214)  C(212)  AND 
CONT  C(105)  C(111)  C(214)  C(212)  C(213) 
SAME  0.01 
CONT  O(161) C(162) C(163) C(164) C(165) C(166) C(167) O(168)  AND 
CONT  O(168) C(167) C(166) C(165) C(164) C(163) C(162) O(161)  AND 
CONT  O(161) C(262) C(263) C(264) C(265) C(266) C(267) O(168)  AND 
CONT  O(168) C(267) C(266) C(265) C(264) C(263) C(262) O(161) 
END                                                                             
;
_cod_data_source_file            ja5b12049_si_002.cif
_cod_data_source_block           2d-M1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4129941