Synthesis of Cryptophane-B: Crystal Structure and Study of Its Complex with Xenon.
Brotin, Thierry; Jeanneau, Erwann; Berthault, Patrick; Léonce, Estelle; Pitrat, Delphine; Mulatier, Jean-Christophe; The Journal of organic chemistry 83 (2018) 14465–14471; doi:10.1021/acs.joc.8b02246

data_4035669
_publ_section_title
;
 Synthesis of Cryptophane-B: Crystal Structure and Study of Its Complex
 with Xenon.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              14465
_journal_page_last               14471
_journal_paper_doi               10.1021/acs.joc.8b02246
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C54 H54 O12, C2 H6 O'
_chemical_formula_sum            'C56 H60 O13'
_chemical_formula_weight         941.08
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                74.380(6)
_cell_angle_beta                 85.802(6)
_cell_angle_gamma                73.462(7)
_cell_formula_units_Z            2
_cell_length_a                   13.0589(10)
_cell_length_b                   13.3601(10)
_cell_length_c                   15.5839(9)
_cell_measurement_reflns_used    14037
_cell_measurement_temperature    150
_cell_measurement_theta_max      67.1605
_cell_measurement_theta_min      2.9419
_cell_volume                     2510.1(3)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED, (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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.079
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8885
_diffrn_reflns_theta_full        67.087
_diffrn_reflns_theta_max         67.087
_diffrn_reflns_theta_min         2.944
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.073
_platon_squeeze_details
;
;
_refine_diff_density_max         1.41
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0134
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         8841
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.0002247
_refine_ls_shift/su_mean         0.0000267
_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: 
 0.104E+04 0.156E+04 780. 182. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1287
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1287
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6471
_reflns_number_total             8885
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.29
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0868
_oxford_refine_ls_scale          4.18(4)
_oxford_reflns_number_all        8841
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            jo8b02246_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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               4035669
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  32,X'S) H   (  31,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  83,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 183,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 483,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 591,X'S) H   ( 593,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  66,X'S) H   ( 662,X'S) H   ( 663,X'S) H   ( 661,X'S) 
RIDE O   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 682,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 692,X'S) H   ( 693,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
VIBRATION 0.0, 0.0050000 = O(67) TO C(68) 
U(IJ)'S  0.0, 0.0050000 = O(67) TO C(68) 
VIBRATION 0.0, 0.005000 = C(69) TO C(68) 
U(IJ)'S  0.0, 0.0050000 = C(69) TO C(68) 
DISTANCE 1.550000 , 0.0050000 = C(68) TO C(69) 
DISTANCE 1.400000 , 0.0050000 = O(67) TO C(68) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;