The distinctively singular self-assembly of a “molecular stair”: observation of a quadrilateral C–H⋯O hydrogen bonding cycle in the crystal structure of a tetracyclic oligo-tetrahydrofuran
Rashid, Showkat; Bhat, Bilal A.; Sen, Saikat; Mehta, Goverdhan; RSC Adv. 5 (2015) 70899–; doi:10.1039/C5RA13749G

data_7221831
_publ_section_title
;
 The distinctively singular self-assembly of a &#x201C;molecular
 stair&#x201D;: observation of a quadrilateral C--H&#x22EF;O hydrogen
 bonding cycle in the crystal structure of a tetracyclic
 oligo-tetrahydrofuran
;
_journal_issue                   87
_journal_name_full               'RSC Adv.'
_journal_page_first              70899
_journal_paper_doi               10.1039/C5RA13749G
_journal_volume                  5
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C10 H12 O5'
_chemical_formula_sum            'C10 H12 O5'
_chemical_formula_weight         212.2
_chemical_name_systematic
;
(1R,2R,6R,8S,10R,14S)-5,7,9,11- tetraoxatetracyclo[6.6.0.0^{2,6}.0^{10,14}]
        tetradecan-4- one
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      154
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-28T16:30:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-09-28 deposited with the CCDC.
2015-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   6.0046(6)
_cell_length_b                   6.0046(6)
_cell_length_c                   45.980(6)
_cell_measurement_reflns_used    815
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7416
_cell_measurement_theta_min      2.8807
_cell_volume                     1435.7(3)
_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
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
'PLATON (Spek, 2003) and CAMERON (Watkin et al., 1993)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.2521318
_diffrn_orient_matrix_UB_12      -0.1037794
_diffrn_orient_matrix_UB_13      -0.0173145
_diffrn_orient_matrix_UB_21      0.1243071
_diffrn_orient_matrix_UB_22      -0.0604384
_diffrn_orient_matrix_UB_23      -0.0258902
_diffrn_orient_matrix_UB_31      -0.0929707
_diffrn_orient_matrix_UB_32      -0.2706268
_diffrn_orient_matrix_UB_33      0.0124296
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            3117
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        70.88
_diffrn_reflns_theta_max         70.88
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88416
_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            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.113
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(4)
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                1454
_reflns_number_total             1752
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5ra13749g1.cif
_cod_data_source_block           platon_acc
_cod_original_cell_volume        1435.7(4)
_cod_database_code               7221831