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_1554982
_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
'C12 H30 N2, C16 H6 O12 S4, 2(C H8 N5), 4(H2 O)'
_chemical_formula_sum            'C30 H60 N12 O16 S4'
_chemical_formula_weight         973.18
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 92.7040(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4741(3)
_cell_length_b                   14.6965(3)
_cell_length_c                   22.6791(4)
_cell_measurement_reflns_used    11631
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.9450
_cell_measurement_theta_min      1.7980
_cell_volume                     4485.96(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
  1 omega   37.00   69.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892  179.0000  120.0000 32

  2 omega  -26.00   70.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892    0.0000 -150.0000 96

  3 omega   -3.00   80.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   38.0000  -90.0000 83

  4 omega  -52.00   32.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -57.0000   90.0000 84

  5 omega  -52.00   33.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892  -50.0000  155.0000 85

  6 omega  -25.00   23.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -99.0000  -90.0000 48

  7 omega  -25.00   23.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -99.0000  120.0000 48

  8 omega  -33.00   51.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   57.0000  -90.0000 84

  9 omega  -25.00   23.00   1.0000   39.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704  -99.0000    0.0000 48

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0291737000
_diffrn_orient_matrix_UB_12      -0.0193237000
_diffrn_orient_matrix_UB_13      0.0220383000
_diffrn_orient_matrix_UB_21      0.0427258000
_diffrn_orient_matrix_UB_22      -0.0222518000
_diffrn_orient_matrix_UB_23      0.0124918000
_diffrn_orient_matrix_UB_31      0.0101081000
_diffrn_orient_matrix_UB_32      0.0382006000
_diffrn_orient_matrix_UB_33      0.0184030000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30126
_diffrn_reflns_theta_full        25.282
_diffrn_reflns_theta_max         29.398
_diffrn_reflns_theta_min         1.798
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.74
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1565
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4783
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.0030364
_refine_ls_shift/su_mean         0.0001225
_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: 
 7.46 -1.29 4.33 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0751
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0684
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4783
_reflns_number_total             5597
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.28
_oxford_diffrn_Wilson_scale      0.86
_oxford_refine_ls_r_factor_ref   0.0769
_oxford_refine_ls_scale          1.590(3)
_oxford_reflns_number_all        5597
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b00779_si_006.cif
_cod_data_source_block           1
_cod_original_cell_volume        4485.97(8)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               1554982
_cell_oxdiff_length_a            13.4702(4)
_cell_oxdiff_length_b            14.7012(4)
_cell_oxdiff_length_c            22.6777(6)
_cell_oxdiff_angle_alpha         89.970(2)
_cell_oxdiff_angle_beta          92.667(2)
_cell_oxdiff_angle_gamma         89.982(2)
_cell_oxdiff_volume              4486.0(2)
_montpellier_reflns_maxres       0.72
_montpellier_reflns_completeness_maxres 90.34
_montpellier_reflns_redundancy_maxres 5.30