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_7703734
_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 Gd5 N16 O22, 3(C H4 O)'
_chemical_formula_sum            'C74 H65 Gd5 N16 O25'
_chemical_formula_weight         2364.67
_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                111.207(3)
_cell_angle_beta                 90.116(4)
_cell_angle_gamma                101.204(3)
_cell_formula_units_Z            2
_cell_length_a                   15.3903(11)
_cell_length_b                   17.2122(14)
_cell_length_c                   20.4239(16)
_cell_measurement_reflns_used    9064
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.41
_cell_volume                     4932.3(7)
_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)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_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  0.1003
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            81851
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.175
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.387
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0905 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.7918.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             2282
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.473
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         19104
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0880P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12387
_reflns_number_total             19104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00210k2.cif
_cod_data_source_block           mo_1203_1_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7703732--7703737.cif.'
_cod_database_code               7703734
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.473
_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-H22A
 0.87 with sigma of 0.01
 H25-H22A
 2.2 with sigma of 0.02
 H19B-H23
 2.2 with sigma of 0.02
 C71-H22A
 2.030565 with sigma of 0.02
 Gd4-H22A
 2.963635 with sigma of 0.02
3. Rigid bond restraints
 O23, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C71, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O23) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Rotating group:
 O19(H19A,H19B)
5.b Aromatic/amide H refined with riding coordinates:
 C54(H54), C3(H3), C22(H22), C7(H7), C10(H10), C52(H52), C40(H40), C41(H41),
 C32(H32), C34(H34), C45(H45), C11(H11), C15(H15), C2(H2), C21(H21), C51(H51),
 C33(H33), C5(H5), C46(H46), C59(H59), C37(H37), C16(H16), C35(H35), C4(H4),
 C29(H29), C24(H24), C56(H56), C58(H58), C26(H26), C28(H28), C27(H27), C57(H57)
5.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C65(H65A,H65B,H65C), C63(H63A,H63B,H63C), C69(H69A,H69B,
 H69C), C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C4AA(H4AA,H4AB,H4AC),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C)
5.d Idealised tetrahedral OH refined as rotating group:
 O23(H23), O24(H24A), O25(H25)
;
_shelx_res_checksum              54163
_shelx_fab_checksum              81385
_olex2_submission_special_instructions 'No special instructions were received'