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_7703732
_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 Dy5 N16 O22, 2(C H4 O)'
_chemical_formula_sum            'C73 H61 Dy5 N16 O24'
_chemical_formula_weight         2358.87
_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                111.135(2)
_cell_angle_beta                 90.178(2)
_cell_angle_gamma                101.146(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3966(8)
_cell_length_b                   17.1849(9)
_cell_length_c                   20.4428(10)
_cell_measurement_reflns_used    9233
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.42
_cell_volume                     4934.2(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            97397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.474
_diffrn_reflns_theta_min         2.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.809
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8555.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             2266
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.575
_refine_diff_density_min         -2.643
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         20341
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+132.5444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.2054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13248
_reflns_number_total             20341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00210k2.cif
_cod_data_source_block           mo_1219_1_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7703732--7703737.cif.'
_cod_database_code               7703732
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.618
_shelx_estimated_absorpt_t_min   0.405
_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
 O22-H22
 0.87 with sigma of 0.01
 H22-H23
 2.2 with sigma of 0.02
 C71-H22
 1.956966 with sigma of 0.02
 Dy1-H22
 2.958828 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C67 \\sim C68: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C67) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C41(H41), C19(H19), C40(H40), C11(H11), C20(H20), C15(H15),
 C59(H59), C52(H52), C16(H16), C51(H51), C45(H45), C3(H3), C2(H2), C37(H37),
 C54(H54), C24(H24), C46(H46), C5(H5), C56(H56), C32(H32), C57(H57), C4(H4),
 C58(H58), C34(H34), C29(H29), C33(H33), C35(H35), C28(H28), C26(H26), C27(H27)
4.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C71(H71A,H71B,H71C), C67(H67A,H67B,H67C), C63(H63A,H63B,
 H63C), C61(H61A,H61B,H61C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C69(H69A,
 H69B,H69C)
4.d Idealised tetrahedral OH refined as rotating group:
 O24(H24A), O23(H23)
;
_shelx_res_checksum              35863
_shelx_fab_checksum              45285
_olex2_submission_special_instructions 'No special instructions were received'