Mitochondria-localizing dicarbohydrazide Ln complexes and their mechanism of in vitro anticancer activity.
Meng, Ting; Liu, Tong; Qin, Qi-Pin; Chen, Zi-Lu; Zou, Hua-Hong; Wang, Kai; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4404–4415; doi:10.1039/d0dt00210k

data_7703737
_publ_section_title
;
 Mitochondria-localizing dicarbohydrazide Ln complexes and their mechanism
 of in vitro anticancer activity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4404
_journal_page_last               4415
_journal_paper_doi               10.1039/d0dt00210k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C71 H53 N16 O22 Tb5, 3(C H4 O)'
_chemical_formula_sum            'C74 H65 N16 O25 Tb5'
_chemical_formula_weight         2373.02
_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   mixed
_audit_creation_date             2019-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-01 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                111.301(2)
_cell_angle_beta                 90.017(2)
_cell_angle_gamma                101.333(2)
_cell_formula_units_Z            2
_cell_length_a                   15.4410(9)
_cell_length_b                   17.2204(10)
_cell_length_c                   20.4129(11)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.40
_cell_volume                     4943.1(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0770
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            105653
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.493
_diffrn_reflns_theta_min         2.148
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0970 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.6955.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.303
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         20401
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+20.4799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14371
_reflns_number_total             20401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00210k2.cif
_cod_data_source_block           mo_1220_8_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7703732--7703737.cif.'
_cod_database_code               7703737
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.633
_shelx_estimated_absorpt_t_min   0.454
_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) groups, All O(H,H) groups
2. Restrained distances
 O20-H20
 0.87 with sigma of 0.01
 H20-H24A
 2.2 with sigma of 0.02
 H19A-H23
 2.2 with sigma of 0.02
 O8-H23
 2 with sigma of 0.02
 H19B_$1-H24_$2
 2.2 with sigma of 0.02
 C71-H20
 1.979718 with sigma of 0.02
 Tb4-H20
 2.919611 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O19(H19A,H19B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C41(H41), C21(H21), C11(H11), C40(H40), C51(H51), C15(H15),
 C29(H29), C10(H10), C16(H16), C54(H54), C22(H22), C26(H26), C28(H28), C59(H59),
  C52(H52), C45(H45), C46(H46), C7(H7), C37(H37), C27(H27), C56(H56), C32(H32),
 C58(H58), C57(H57), C2(H2), C5(H5), C35(H35), C33(H33), C34(H34), C3(H3),
 C4(H4)
4.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C61(H61A,H61B,H61C), C65(H65A,H65B,
 H65C), C69(H69A,H69B,H69C), C73(H73A,H73B,H73C), C63(H63A,H63B,H63C), C74(H74A,
 H74B,H74C), C72(H72A,H72B,H72C)
4.d Idealised tetrahedral OH refined as rotating group:
 O25(H25), O24(H24A), O23(H23)
;
_shelx_res_checksum              94021
_shelx_fab_checksum              44870
_olex2_submission_special_instructions 'No special instructions were received'