Construction of cross-layer linked G-octamer via conformational control: stable G-quadruplex in H-bond competitive solvent
Shi, Xiaodong; He, Ying; Zhang, Yanbin; Wojtas, Lukasz; Ahkmedov, Novruz G.; Thai, David; Wang, Heng; Li, Xiaopeng; Guo, Hao; Chemical Science  (2019) –; doi:10.1039/C9SC00190E

data_1550706
_publ_section_title
;
 Construction of cross-layer linked G-octamer via conformational control:
 stable G-quadruplex in H-bond competitive solvent
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00190E
_journal_year                    2019
_chemical_formula_sum            'C452.15 H656.6 Cl6.5 K2 N86 O94 Si16'
_chemical_formula_weight         9559.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-10-04 deposited with the CCDC.    2019-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.4610(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.320(3)
_cell_length_b                   22.277(2)
_cell_length_c                   44.399(4)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.9
_cell_measurement_theta_min      2.25
_cell_volume                     29039(5)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Pilatus3 X CdTe 1M'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.44281
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            734274
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        15.408
_diffrn_reflns_theta_max         16.169
_diffrn_reflns_theta_min         0.813
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.030
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs-2016/2, Bruker AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       plate
_exptl_crystal_F_000             10192
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 37612 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6719
_refine_ls_number_reflns         115388
_refine_ls_number_restraints     12939
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0953
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2073P)^2^+4.5400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2614
_refine_ls_wR_factor_ref         0.2830
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                92579
_reflns_number_total             115388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00190e2.cif
_cod_data_source_block           HY_II_207_6
_cod_original_cell_volume        29038(4)
_cod_original_formula_sum        'C452.15 H656.60 Cl6.50 K2 N86 O94 Si16'
_cod_database_code               1550706
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              8922