Synthesis and Solid-State Self-Assembly of Polyphenols
Venkataramanan, Balasubramaniam; James, Wong Ling Guan; Vittal, Jagadese J.; Suresh, Valiyaveettil; Crystal Growth & Design 4 (2004) 553–; doi:10.1021/cg0341508

data_4511620
_publ_section_title
;
 Synthesis and Solid-State Self-Assembly of Polyphenols
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              553
_journal_paper_doi               10.1021/cg0341508
_journal_volume                  4
_journal_year                    2004
_chemical_formula_sum            'C19 H24 O9'
_chemical_formula_weight         396.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.083(2)
_cell_angle_beta                 88.217(2)
_cell_angle_gamma                87.818(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3808(7)
_cell_length_b                   10.8134(9)
_cell_length_c                   11.1500(9)
_cell_measurement_reflns_used    2648
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.4
_cell_volume                     975.47(14)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15063
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.6663
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular shape, cut'
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                4116
_reflns_number_total             5639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0341508si20040303_042541.cif
_cod_data_source_block           189a
_cod_depositor_comments
;
The original CIF contained some information in plain text format that 
was 'glued' to  the value of '_refine_diff_density_rms' tag upon deposition.
The information was removed and stored here for further investigation. The 
following lines were extracted (delimited by #--):
 Hydrogen bonds with  H..A < r(A) + 2.000 Angstroms  and  <DHA > 110 deg. 

 D-H         d(D-H)   d(H..A)   <DHA    d(D..A)   A

 O2-H2       0.88(2)  2.03(2)  147(2)   2.806(1)  O3 [ -x+2, -y+1, -z+1 ]
 O2-H2       0.88(2)  2.30(2)  111(2)   2.746(1)  O3
 O3-H3       0.91(2)  1.72(2)  171(2)   2.619(2)  O2S
 O4-H4       0.91(2)  1.77(2)  169(2)   2.659(1)  O1S [ x, y-1, z+1 ]
 O5-H5       0.91(2)  1.89(2)  160(2)   2.762(1)  O4 [ -x+1, -y, -z+2 ]
 O1S-H1SA    0.87(2)  1.89(2)  169(2)   2.742(2)  O4S [ x, y, z-1 ]
 O1S-H1SB    0.91(2)  1.85(3)  163(2)   2.730(2)  O3S
 O2S-H2SA    0.85(3)  1.94(3)  166(2)   2.772(2)  O1S [ -x+2, -y+1, -z+1 ]
 O2S-H2SB    0.94(3)  1.87(3)  167(2)   2.797(2)  O4S
 O3S-H3SA    0.92(2)  1.87(2)  166(2)   2.778(2)  O1
 O3S-H3SA    0.92(2)  2.61(2)  118(3)   3.151(2)  O2
 O3S-H3SB    0.83(3)  2.31(2)  129(3)   2.909(2)  O5 [ -x+1, -y+1, -z+1 ]
 O4S-H4SA    0.99(3)  1.78(3)  176(2)   2.765(2)  O3S [ -x+1, -y+1, -z+1 ]
Antanas Vaitkus,
2015-02-28

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4511620