Delivering the cell-impermeable DNA ‘light-switching’ Ru(ii) complexes preferentially into live-cell nucleus via an unprecedented ion-pairing method
Zhu, Ben-Zhan; Chao, Xi-Juan; Huang, Chun-Hua; Li, Yan; Chem. Sci. 7 (2016) 4016–; doi:10.1039/C5SC03796D

data_1543044
_publ_section_title
;
 Delivering the cell-impermeable DNA &#x2018;light-switching&#x2019;
 Ru(ii) complexes preferentially into live-cell nucleus via an
 unprecedented ion-pairing method
;
_journal_issue                   7
_journal_name_full               'Chem. Sci.'
_journal_page_first              4016
_journal_paper_doi               10.1039/C5SC03796D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C36 H24 N6 Ru, 2(C6 Cl5 O), C2 H3 N, 6(H2 O)'
_chemical_formula_sum            'C50 H39 Cl10 N7 O8 Ru'
_chemical_formula_weight         1321.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-02-02 deposited with the CCDC.
2016-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7707(5)
_cell_length_b                   12.8886(3)
_cell_length_c                   24.1907(6)
_cell_measurement_reflns_used    24370
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.4850
_cell_measurement_theta_min      3.3740
_cell_volume                     5228.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.4713
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -83.00   -1.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.2847  -57.0000   30.0000 82

  2 omega  -49.00   13.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.2847  -38.0000   60.0000 62

  3 omega -102.00  -56.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.2847 -178.0000    0.0000 46

  4 omega  -66.00  -39.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -       11.8941  178.0000 -180.0000 27

  5 omega  -97.00  -42.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.1285 -178.0000 -120.0000 55

  6 omega   53.00  100.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -       11.8941 -178.0000  -60.0000 47

  7 omega  -88.00  -63.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.1285  -38.0000  -60.0000 25

  8 omega  -88.00   14.00   1.0000    2.8600
omega____ theta____ kappa____ phi______ frames
    -      -12.1285  -38.0000 -150.0000 102
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0372854000
_diffrn_orient_matrix_UB_12      0.0250021000
_diffrn_orient_matrix_UB_13      0.0037167000
_diffrn_orient_matrix_UB_21      0.0198329000
_diffrn_orient_matrix_UB_22      -0.0480377000
_diffrn_orient_matrix_UB_23      -0.0039562000
_diffrn_orient_matrix_UB_31      0.0020927000
_diffrn_orient_matrix_UB_32      0.0098225000
_diffrn_orient_matrix_UB_33      -0.0288185000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51902
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 4498 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         10230
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+5.9132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                9674
_reflns_number_total             10230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03796d2.cif
_cod_data_source_block           pcpruop
_cod_depositor_comments          'Adding full bibliography for 1543044.cif.'
_cod_database_code               1543044
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1 Ru1'
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.880
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4A,H4B,O5,H5A,H5B,O6,H6A,H6B,O3,H3A,H3B,O7,H7A,H7B,O8,H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'