Synthesis of polyyne rotaxanes.
Movsisyan, Levon D.; Kondratuk, Dmitry V.; Franz, Michael; Thompson, Amber L.; Tykwinski, Rik R.; Anderson, Harry L.; Organic letters 14 (2012) 3424–3426; doi:10.1021/ol301392t

data_1508579
_publ_section_title
;
 Synthesis of polyyne rotaxanes.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3424
_journal_page_last               3426
_journal_paper_doi               10.1021/ol301392t
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C98 H126, C42 H42 N2 O4, 4(C H4 O)'
_chemical_formula_sum            'C144 H184 N2 O8'
_chemical_formula_weight         2071.05
_chemical_melting_point          ?
_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_creation_date             12-05-15
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                97.176(3)
_cell_angle_beta                 102.427(3)
_cell_angle_gamma                92.395(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3026(6)
_cell_length_b                   19.4275(9)
_cell_length_c                   26.7908(10)
_cell_measurement_reflns_used    23335
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.1028
_cell_measurement_theta_min      1.5232
_cell_volume                     6691.7(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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 0.963
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device
;
CrystalLogic Kappa (3 circle)
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            127381
_diffrn_reflns_theta_full        25.286
_diffrn_reflns_theta_max         30.103
_diffrn_reflns_theta_min         1.523
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.29
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1507
_refine_ls_number_reflns         18295
_refine_ls_number_restraints     776
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0950
_refine_ls_shift/su_max          0.0025315
_refine_ls_shift/su_mean         0.0000915
_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: 
 0.418E+04 0.704E+04 0.433E+04 0.180E+04 406. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2666
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.2665
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              27
_reflns_limit_k_min              -28
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                15230
_reflns_number_total             37260
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.41
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_r_factor_ref   0.1055
_oxford_refine_ls_scale          3.50(4)
_oxford_reflns_number_all        18297
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0156
_cod_duplicate_entry             1507864
_cod_data_source_file            ol301392t_si_001.cif
_cod_data_source_block           1b
_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
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1508579
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
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   ( 229,X'S) H   (2291,X'S) H   (2292,X'S) H   (2293,X'S) 
RIDE C   ( 228,X'S) H   (2282,X'S) H   (2281,X'S) H   (2283,X'S) 
RIDE C   ( 230,X'S) H   (2302,X'S) H   (2301,X'S) H   (2303,X'S) 
RIDE C   (  32,X'S) H   ( 322,X'S) H   ( 321,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,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   ( 483,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 493,X'S) H   ( 492,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   ( 683,X'S) H   ( 682,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 693,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 703,X'S) H   ( 702,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 723,X'S) H   ( 722,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   ( 902,X'S) H   ( 901,X'S) H   ( 903,X'S) 
RIDE C   (  92,X'S) H   ( 922,X'S) H   ( 921,X'S) H   ( 923,X'S) 
RIDE C   (  93,X'S) H   ( 932,X'S) H   ( 931,X'S) H   ( 933,X'S) 
RIDE C   (  94,X'S) H   ( 942,X'S) H   ( 941,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   (1083,X'S) H   (1082,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1093,X'S) H   (1092,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1103,X'S) H   (1102,X'S) 
RIDE C   ( 208,X'S) H   (2081,X'S) H   (2082,X'S) H   (2083,X'S) 
RIDE C   ( 209,X'S) H   (2091,X'S) H   (2093,X'S) H   (2092,X'S) 
RIDE C   ( 210,X'S) H   (2101,X'S) H   (2103,X'S) H   (2102,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1123,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1133,X'S) H   (1132,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   (1322,X'S) H   (1321,X'S) H   (1323,X'S) 
RIDE C   ( 133,X'S) H   (1332,X'S) H   (1331,X'S) H   (1333,X'S) 
RIDE C   ( 134,X'S) H   (1342,X'S) H   (1341,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   (1622,X'S) H   (1621,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   (1662,X'S) H   (1661,X'S) 
RIDE C   ( 167,X'S) H   (1671,X'S) H   (1672,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   (2652,X'S) H   (2651,X'S) 
RIDE C   ( 266,X'S) H   (2661,X'S) H   (2662,X'S) 
RIDE C   ( 267,X'S) H   (2671,X'S) H   (2672,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 O   ( 301,X'S) H   (3011,X'S) 
RIDE C   ( 302,X'S) H   (3021,X'S) H   (3023,X'S) H   (3022,X'S) 
RIDE O   ( 303,X'S) H   (3031,X'S) 
RIDE C   ( 304,X'S) H   (3042,X'S) H   (3043,X'S) H   (3041,X'S) 
RIDE O   ( 305,X'S) H   (3051,X'S) 
RIDE C   ( 306,X'S) H   (3062,X'S) H   (3063,X'S) H   (3061,X'S) 
RIDE O   ( 307,X'S) H   (3071,X'S) 
RIDE C   ( 308,X'S) H   (3083,X'S) H   (3082,X'S) H   (3081,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME  C(23)  C(27)  C(28)  C(29)  C(30) AND 
CONT  C(23)  C(27)  C(29)  C(30) C(28)  AND 
CONT  C(23)  C(27)  C(30) C(28)  C(29)  AND 
CONT  C(23)  C(27)  C(228)  C(229)  C(230) AND 
CONT  C(23)  C(27)  C(229)  C(230) C(228)  AND 
CONT  C(23)  C(27)  C(230) C(228)  C(229)  AND 
CONT  C(103) C(107) C(108) C(109) C(110)  AND 
CONT  C(103) C(107) C(109) C(110) C(108) AND 
CONT  C(103) C(107) C(110) C(108) C(109) AND 
CONT  C(103) C(107) C(208) C(209) C(210)  AND 
CONT  C(103) C(107) C(209) C(210) C(208) AND 
CONT  C(103) C(107) C(210) C(208) C(209) 
SIMU  0.01   C(23)  C(27)  C(28)  C(29)  C(30) AND 
CONT  C(23)  C(27)  C(29)  C(30) C(28)  AND 
CONT  C(23)  C(27)  C(30) C(28)  C(29)  AND 
CONT  C(23)  C(27)  C(228)  C(229)  C(230) AND 
CONT  C(23)  C(27)  C(229)  C(230) C(228)  AND 
CONT  C(23)  C(27)  C(230) C(228)  C(229)  AND 
CONT  C(103) C(107) C(108) C(109) C(110)  AND 
CONT  C(103) C(107) C(109) C(110) C(108) AND 
CONT  C(103) C(107) C(110) C(108) C(109) AND 
CONT  C(103) C(107) C(208) C(209) C(210)  AND 
CONT  C(103) C(107) C(209) C(210) C(208) AND 
CONT  C(103) C(107) C(210) C(208) C(209) 
DELU  0.01   C(23)  C(27)  C(28)  C(29)  C(30) AND 
CONT  C(23)  C(27)  C(29)  C(30) C(28)  AND 
CONT  C(23)  C(27)  C(30) C(28)  C(29)  AND 
CONT  C(23)  C(27)  C(228)  C(229)  C(230) AND 
CONT  C(23)  C(27)  C(229)  C(230) C(228)  AND 
CONT  C(23)  C(27)  C(230) C(228)  C(229)  AND 
CONT  C(103) C(107) C(108) C(109) C(110)  AND 
CONT  C(103) C(107) C(109) C(110) C(108) AND 
CONT  C(103) C(107) C(110) C(108) C(109) AND 
CONT  C(103) C(107) C(208) C(209) C(210)  AND 
CONT  C(103) C(107) C(209) C(210) C(208) AND 
CONT  C(103) C(107) C(210) C(208) C(209) 
SAME  C(158) O(161) C(162) C(163) C(164) 
CONT  C(165) C(166) C(167) O(168) C(184) AND 
CONT  C(184) O(168) C(167) C(166) C(165) 
CONT  C(164) C(163) C(162) O(161) C(158) AND 
CONT  C(158) O(261) C(262) C(263) C(264) 
CONT  C(265) C(266) C(267) O(168) C(184) AND 
CONT  C(184) O(168) C(267) C(266) C(265) 
CONT  C(264) C(263) C(262) O(261) C(158) 
SIMU  0.01   C(158) O(161) C(162) C(163) C(164) 
CONT  C(165) C(166) C(167) O(168) C(184) AND 
CONT  C(184) O(168) C(167) C(166) C(165) 
CONT  C(164) C(163) C(162) O(161) C(158) AND 
CONT  C(158) O(261) C(262) C(263) C(264) 
CONT  C(265) C(266) C(267) O(168) C(184) AND 
CONT  C(184) O(168) C(267) C(266) C(265) 
CONT  C(264) C(263) C(262) O(261) C(158) 
DELU  0.01   C(158) O(161) C(162) C(163) C(164) 
CONT  C(165) C(166) C(167) O(168) C(184) AND 
CONT  C(184) O(168) C(167) C(166) C(165) 
CONT  C(164) C(163) C(162) O(161) C(158) AND 
CONT  C(158) O(261) C(262) C(263) C(264) 
CONT  C(265) C(266) C(267) O(168) C(184) AND 
CONT  C(184) O(168) C(267) C(266) C(265) 
CONT  C(264) C(263) C(262) O(261) C(158) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;