New "pyrene box" cages for adaptive guest conformations.
Dumitrescu, Dan; Dumitru, Florina; Legrand, Yves-Marie; Petit, Eddy; van der Lee, Arie; Barboiu, Mihail; Organic letters 17 (2015) 2178–2181; doi:10.1021/acs.orglett.5b00779

data_1554988
_publ_section_title
;
 New &quot;pyrene box&quot; cages for adaptive guest conformations.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              2178
_journal_page_last               2181
_journal_paper_doi               10.1021/acs.orglett.5b00779
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         '2(C12 H30 N2), C16 H6 O12 S4, 2(H2 O)'
_chemical_formula_sum            'C40 H69.97 N4 O14 S4'
_chemical_formula_weight         959.25
_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     iterative
_cell_angle_alpha                111.587(16)
_cell_angle_beta                 100.691(16)
_cell_angle_gamma                109.004(13)
_cell_formula_units_Z            2
_cell_length_a                   11.2634(18)
_cell_length_b                   15.966(2)
_cell_length_c                   16.009(4)
_cell_measurement_reflns_used    8004
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.0640
_cell_measurement_theta_min      1.7110
_cell_volume                     2373.6(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details
;
  1 omega   -2.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7806   57.0000 -150.0000 87

  2 omega  -52.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7806  -57.0000  -30.0000 87

  3 omega  -54.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7806    0.0000 -180.0000 142

  4 omega  -84.00  -30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7181  143.0000 -150.5527 54

  5 omega  -82.00  -28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7181  140.0000   17.8968 54

  6 omega  -24.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7181 -100.0000  150.0000 47

  7 omega   34.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7806  179.0000 -150.0000 51

  8 omega   -2.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7806   57.0000  -30.0000 87

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0644345000
_diffrn_orient_matrix_UB_12      -0.0053797000
_diffrn_orient_matrix_UB_13      0.0016443000
_diffrn_orient_matrix_UB_21      -0.0187824000
_diffrn_orient_matrix_UB_22      -0.0027174000
_diffrn_orient_matrix_UB_23      -0.0461010000
_diffrn_orient_matrix_UB_31      -0.0234156000
_diffrn_orient_matrix_UB_32      -0.0526852000
_diffrn_orient_matrix_UB_33      -0.0215188000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30663
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         29.136
_diffrn_reflns_theta_min         1.949
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'big plate'
_exptl_crystal_F_000             1027.946
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         8405
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.0004293
_refine_ls_shift/su_mean         0.0000210
_refine_ls_structure_factor_coef F
_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: 
 3.26 -11.9 -3.27 -4.79 -3.50 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0545
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0454
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              -21
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8405
_reflns_number_total             11085
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.52
_oxford_diffrn_Wilson_scale      0.32
_oxford_refine_ls_r_factor_ref   0.0729
_oxford_refine_ls_scale          2.930(4)
_oxford_reflns_number_all        11050
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b00779_si_008.cif
_cod_data_source_block           1
_cod_original_cell_volume        2373.5(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1554988
_cell_oxdiff_length_a            11.2659(5)
_cell_oxdiff_length_b            15.9660(7)
_cell_oxdiff_length_c            16.0025(7)
_cell_oxdiff_angle_alpha         111.674(4)
_cell_oxdiff_angle_beta          100.737(4)
_cell_oxdiff_angle_gamma         109.046(4)
_cell_oxdiff_volume              2369.19(18)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 86.48
_montpellier_reflns_redundancy_maxres 2.77