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_1554981
_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
'3(C12 H30 N2), 2(C16 H6 O12 S4), 2(C H7 N4), 2(H2 O)'
_chemical_formula_sum            'C70 H120 N14 O26 S8'
_chemical_formula_weight         1830.36
_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                80.344(4)
_cell_angle_beta                 63.999(4)
_cell_angle_gamma                78.993(3)
_cell_formula_units_Z            1
_cell_length_a                   13.0106(5)
_cell_length_b                   13.1402(6)
_cell_length_c                   14.3888(7)
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    175
_cell_measurement_theta_max      29.2860
_cell_measurement_theta_min      1.7610
_cell_volume                     2160.42(18)
_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 0.851
_diffrn_measurement_details
;
  1 omega  -56.00   39.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -       15.6454  -19.0000 -150.0000 95

  2 omega  -10.00   52.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -       15.6454   77.0000  150.0000 62

  3 omega    0.00   85.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -       15.6454   38.0000   30.0000 85

  4 omega  -24.00   10.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -       15.6454  -99.0000 -150.0000 34

  5 omega   22.00   58.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -       15.6454   57.0000   90.0000 36

  6 omega  -25.00   22.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -      -16.4267  -99.0000   30.0000 47

  7 omega  -59.00  -25.00   1.0000    9.8000
omega____ theta____ kappa____ phi______ frames
    -      -16.4267  110.0000 -168.0000 34

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0398396000
_diffrn_orient_matrix_UB_12      0.0265577000
_diffrn_orient_matrix_UB_13      0.0435861000
_diffrn_orient_matrix_UB_21      0.0251343000
_diffrn_orient_matrix_UB_22      -0.0321022000
_diffrn_orient_matrix_UB_23      0.0314771000
_diffrn_orient_matrix_UB_31      0.0390639000
_diffrn_orient_matrix_UB_32      0.0362741000
_diffrn_orient_matrix_UB_33      -0.0120455000
_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  0.027
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19044
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         29.210
_diffrn_reflns_theta_min         1.582
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96721
_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            yellowish
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.44
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0683
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8229
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0009077
_refine_ls_shift/su_mean         0.0000497
_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: 
 10.0 -0.763E-01 7.52 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0645
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0550
_reflns_limit_h_max              17
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8229
_reflns_number_total             9947
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.33
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0483
_oxford_refine_ls_scale          3.253(4)
_oxford_reflns_number_all        9946
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ol5b00779_si_007.cif
_cod_data_source_block           1
_cod_original_cell_volume        2160.43(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               1554981
_cell_oxdiff_length_a            13.0106(5)
_cell_oxdiff_length_b            13.1402(5)
_cell_oxdiff_length_c            14.3888(7)
_cell_oxdiff_angle_alpha         80.345(4)
_cell_oxdiff_angle_beta          63.999(4)
_cell_oxdiff_angle_gamma         78.993(3)
_cell_oxdiff_volume              2160.43(16)
_montpellier_reflns_maxres       0.73
_montpellier_reflns_completeness_maxres 85.09
_montpellier_reflns_redundancy_maxres 1.91