Luminescent ruthenium polypyridyl complexes with extended 'dppz' like ligands as DNA targeting binders and cellular agents.
Poulsen, Bjørn C; Estalayo-Adrián, Sandra; Blasco, Salvador; Bright, Sandra A.; Kelly, John M.; Williams, D. Clive; Gunnlaugsson, Thorfinnur; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18208–18220; doi:10.1039/c6dt03792e

data_7040988
_publ_section_title
;
 Luminescent ruthenium polypyridyl complexes with extended 'dppz' like
 ligands as DNA targeting binders and cellular agents.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18208
_journal_page_last               18220
_journal_paper_doi               10.1039/c6dt03792e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C41 H24 N14 Ru, 2(Cl)'
_chemical_formula_sum            'C41 H24 Cl2 N14 Ru'
_chemical_formula_weight         884.70
_chemical_melting_point_gt       250
_chemical_name_systematic
'Bis(1,4,5,8-tetraazaphenanthrene)(3-methyl-pyrazino[2,3-h]dipyrido[3,2-a:2?,3?-c]phenazine)ruthenium(II) chloride '
_chemical_properties_physical    ', Light-sensitive,Photo-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                63.55(6)
_cell_angle_beta                 80.88(6)
_cell_angle_gamma                88.05(6)
_cell_formula_units_Z            4
_cell_length_a                   13.41(5)
_cell_length_b                   20.75(7)
_cell_length_c                   21.49(8)
_cell_measurement_reflns_used    3832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.31
_cell_volume                     5282(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1647
_diffrn_reflns_av_unetI/netI     0.2032
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40213
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        20.698
_diffrn_reflns_theta_max         20.698
_diffrn_reflns_theta_min         1.539
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1059 before and 0.0793 after correction.
The Ratio of minimum to maximum transmission is 0.7372.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       prism
_exptl_crystal_F_000             1782
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         10142
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.2165
_refine_ls_R_factor_gt           0.0992
_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^)+(0.1896P)^2^+1.6332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2605
_refine_ls_wR_factor_ref         0.3361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             10142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03792e2.cif
_cod_data_source_block           sal49s_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>250' was changed to
'250' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7040988--7040989.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C82 H47 Cl4 N28 Ru2'
_cod_original_formula_weight         1768.41
_cod_original_formula_moiety         'C41 H23 N14 Ru, C41 H24 N14 Ru, 4(Cl)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5282(33)
_cod_database_code               7040988
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.910
_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
2. Restrained distances
 N9-C28 \\sim N8-C25
 with sigma of 0.02
 N8-C24 \\sim N9-C29
 with sigma of 0.02
3. Rigid bond restraints
 C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C52
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N23, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C80, C81
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N22, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C74, C75
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C73, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C79) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C55) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C59) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C63) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C67) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C47) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C33)
\\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.1
Uanis(C2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.1
Uanis(C14) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C36) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C9(H9), C13(H13), C23(H23), C19(H19), C4(H4), C3(H3), C2(H2),
 C8(H8), C24(H24), C27(H27), C30(H30), C33(H33), C36(H36), C37(H37), C40(H40),
 C43(H43), C44(H44), C45(H45), C59(H59), C60(H60), C61(H61), C54(H54), C50(H50),
  C49(H49), C71(H71), C70(H70), C68(H68), C67(H67), C65(H65), C64(H64),
 C75(H75), C74(H74), C81(H81), C80(H80), C78(H78), C77(H77), C26(H26), C29(H29),
  C34(H34), C39(H39)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              93441
_shelx_fab_checksum              73384
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method 'methanol, diethylether'