A cytotoxic nitrido-osmium(VI) complex induces caspase-mediated apoptosis in HepG2 cancer cells.
Huang, Wan-Qiong; Wang, Chuan-Xian; Liu, Tao; Li, Zi-Xin; Pan, Chen; Chen, Yun-Zhou; Lian, Xin; Man, Wai-Lun; Ni, Wen-Xiu; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17173–17182; doi:10.1039/d0dt02715d

data_7705697
_publ_section_title
;
 A cytotoxic nitrido-osmium(VI) complex induces caspase-mediated apoptosis
 in HepG2 cancer cells.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17173
_journal_page_last               17182
_journal_paper_doi               10.1039/d0dt02715d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(C18 H14 Cl N3 O2 Os), 3(C H2 Cl2)'
_chemical_formula_sum            'C39 H34 Cl8 N6 O4 Os2'
_chemical_formula_weight         1314.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-10 deposited with the CCDC.	2020-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.544(3)
_cell_angle_beta                 87.869(3)
_cell_angle_gamma                84.639(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1575(3)
_cell_length_b                   12.0799(5)
_cell_length_c                   12.5607(5)
_cell_measurement_reflns_used    4202
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6790
_cell_measurement_theta_min      10.1580
_cell_volume                     1059.54(8)
_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      173.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6725
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.451
_diffrn_reflns_theta_min         3.748
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       block
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.973
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0718P)^2^+6.0237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3877
_reflns_number_total             3935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02715d2.cif
_cod_data_source_block           082216a_beyond
_cod_depositor_comments          'Adding full bibliography for 7705697.cif.'
_cod_database_code               7705697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.140
_shelx_estimated_absorpt_t_min   0.038
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C5-C4 = C4-C3 = C3-C2 = C2-C1
 1.39 with sigma of 0.02
 C5-N1 = C1-N1
 1.35 with sigma of 0.02
3. Rigid bond restraints
 N1, C5, C4, C3, C2, C1, N1B, C5B, C4B, C3B, C2B, C1B
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
N1 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim N1B \\sim C5B \\sim C4B
\\sim C3B \\sim C2B \\sim C1B: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
O2 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O2) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq:
with sigma of 0.04 and sigma for terminal atoms of 0.12
5. Rigid body (RIGU) restrains
 O2, C18, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Same fragment restrains
{N1, C5, C4, C3, C2, C1} sigma for 1-2: 0.02, 1-3: 0.04
as
{N1B, C5B, C4B, C3B, C2B, C1B}
7. Others
 Sof(N1B)=Sof(C5B)=Sof(H5B)=Sof(C4B)=Sof(H4B)=Sof(C3B)=Sof(H3B)=Sof(C2B)=
 Sof(H2B)=Sof(C1B)=Sof(H1B)=1-FVAR(1)
 Sof(N1)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(C2)=Sof(H2)=
 Sof(C1)=Sof(H1)=FVAR(1)
 Fixed Sof: Cl4(0.5) Cl5(0.5) C20(0.5) H20A(0.5) H20B(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C5(H5), C4(H4), C3(H3), C2(H2), C1(H1), C5B(H5B), C4B(H4B), C3B(H3B),
  C2B(H2B), C1B(H1B)
;
_shelx_res_checksum              90600
_olex2_submission_special_instructions 'No special instructions were received'