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_7221832
_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 unk
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C10 H14 O4'
_chemical_formula_sum            'C10 H14 O4'
_chemical_formula_weight         198.21
_chemical_name_systematic
;
        (1r,2R,6S,8r,10R,14S)-5,7,9,11-
        tetraoxatetracyclo[6.6.0.0^2,6^.0^10,14^]tetradecane
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-12T22:16:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-07-12 deposited with the CCDC.
2015-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.096(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.420(5)
_cell_length_b                   5.899(3)
_cell_length_c                   15.377(8)
_cell_measurement_reflns_used    2178
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.85
_cell_measurement_theta_min      2.66
_cell_volume                     942.8(8)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_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      291(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3444
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.8463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'see text above'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         967
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.282
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.5510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.1933
_reflns_number_gt                878
_reflns_number_total             967
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5ra13749g1.cif
_cod_data_source_block           tetracyclic_oligoacetal_4_cif
_cod_original_cell_volume        942.7(8)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7221832