Determination of a complex crystal structure in the absence of single crystals: analysis of powder X-ray diffraction data, guided by solid-state NMR and periodic DFT calculations, reveals a new 2'-deoxyguanosine structural motif
Colan E. Hughes; G. N. Manjunatha Reddy; Stefano Masiero; Steven P. Brown; P. Andrew Williams; Kenneth D. M. Harris; Chemical Science 8 (2017) 3971–3979; doi:10.1039/c7sc00587c

data_1547319
_publ_section_title
;
 Determination of a complex crystal structure in the absence of single
 crystals: analysis of powder X-ray diffraction data, guided by
 solid-state NMR and periodic DFT calculations, reveals a new
 2'-deoxyguanosine structural motif
;
_journal_name_full               'Chemical Science'
_journal_page_first              3971
_journal_page_last               3979
_journal_paper_doi               10.1039/c7sc00587c
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C30 H49 N5 O6'
_chemical_formula_sum            'C30 H49 N5 O6'
_chemical_formula_weight         575.75
_chemical_name_common            dG(C10)2
_chemical_name_systematic        3',5'-bis-O-decanoyl-2'-deoxyguanosine
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 97.491(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   8.3072(7)
_cell_length_b                   7.8052(10)
_cell_length_c                   25.7246(27)
_cell_volume                     1653.7(3)
_computing_structure_refinement  GSAS
_diffrn_ambient_temperature      294
_diffrn_radiation_polarisn_ratio 0.55
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     1.5406
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01707
_pd_meas_2theta_range_max        50.00527
_pd_meas_2theta_range_min        3.0
_pd_meas_number_of_points        2755
_pd_phase_name
'from C:/Users/colan/Documents/CASTEP/dGC10/Conf C/Opt/dGC10_E.cif'
_pd_proc_2theta_range_inc        0.01707
_pd_proc_2theta_range_max        50.02392
_pd_proc_2theta_range_min        3.01864
_pd_proc_info_datetime           2016-08-16T12:37:50
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 36 terms.
 Shifted Chebyshev function of 1st kind
      1:    12592.5     2:   -14617.3     3:    6625.64     4:   -3575.60    
      5:    2794.90     6:   -2823.66     7:    2690.04     8:   -2088.00    
      9:    1071.62    10:   -181.454    11:    202.977    12:   -492.012    
     13:    442.357    14:   -353.955    15:    211.950    16:    68.0129    
     17:   -227.257    18:    188.320    19:   -61.2709    20:   -27.5406    
     21:    4.79306    22:    78.7039    23:   -115.802    24:    96.5546    
     25:   -39.3211    26:   -28.5510    27:    60.4133    28:   -51.8408    
     29:    41.0777    30:   -37.2673    31:    33.4308    32:   -40.7213    
     33:    49.0372    34:   -42.7856    35:    32.6701    36:   -19.6815    
;
_pd_proc_ls_peak_cutoff          0.00250
_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =  472.470 #2(GV)   =    0.000 #3(GW)   =    4.216
 #4(GP)   =    0.000 #5(LX)   =    0.000 #6(LY)   =   73.926
 #7(S/L)  =   0.0044 #8(H/L)  =   0.0174
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.244 #15(L22) =   -0.378 #16(L33) =   -0.054
 #17(L12) =    0.144 #18(L13) =    0.099 #19(L23) =   -0.017
 Peak tails are ignored  where the intensity is below 0.0025 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0115
_pd_proc_ls_prof_wR_expected     0.0096
_pd_proc_ls_prof_wR_factor       0.0156
_pd_proc_number_of_points        2755
_pd_spec_mounting                ' ?'
_refine_ls_goodness_of_fit_all   1.69
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_restraints     306
_refine_ls_R_Fsqd_factor         0.17052
_refine_ls_shift/su_max          1.03
_refine_ls_shift/su_mean         0.12
_reflns_d_resolution_high        1.823
_reflns_d_resolution_low         25.505
_reflns_limit_h_max              4
_reflns_limit_h_min              0
_reflns_limit_k_max              4
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_total             340
_cod_data_source_file            SC-008-C7SC00587C-s002.cif
_cod_data_source_block           1
_cod_original_cell_volume        1653.74(17)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1547319