Tuning the allosteric sequestration of anticancer drugs for developing cooperative nano-antidotes.
Wang, Weikun; Finnegan, Tyler J.; Lei, Zhiquan; Zhu, Xingrong; Moore, Curtis E.; Shi, Kejia; Badjić, Jovica D; Chemical communications (Cambridge, England) 56 (2020) 1271–1274; doi:10.1039/c9cc09373g

data_7125668
_publ_section_title
;
 Tuning the allosteric sequestration of anticancer drugs for developing
 cooperative nano-antidotes.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1271
_journal_page_last               1274
_journal_paper_doi               10.1039/c9cc09373g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C84 H60 N6 O24, 0.27(C2 H6 O S), 0.48(C H2 Cl2)'
_chemical_formula_sum            'C85.01 H62.56 Cl0.94 N6 O24.27 S0.27'
_chemical_formula_weight         1598.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-02 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.839(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0085(6)
_cell_length_b                   24.5621(10)
_cell_length_c                   16.7777(7)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.193
_cell_measurement_theta_min      2.941
_cell_volume                     5354.2(4)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            242352
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.2269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0628 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.8637. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_description       Block
_exptl_crystal_F_000             1658
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         10767
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0879
_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^)+(0.1481P)^2^+8.6725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2481
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8696
_reflns_number_total             10767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09373g2.cif
_cod_data_source_block           Badjic_WK_GABA
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7125668.cif.
;
_cod_database_code               7125668
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C40B-C39B = N3B-C39B = C40B-C41B
 1.5 with sigma of 0.02
 Cl1S-C1S = Cl2S-C1S
 1.8 with sigma of 0.02
 O12B-C42B = O11B-C42B
 1.3 with sigma of 0.02
 C41B-C42B
 1.54 with sigma of 0.02
 O13-O14
 2.1 with sigma of 0.02
 O11B-O12B
 2.2 with sigma of 0.02
 S1S-O1S
 1.5 with sigma of 0.02
 C4S-S1S
 1.8 with sigma of 0.02
 S1S-C3S
 1.8 with sigma of 0.02
 Cl3S-C2S
 1.8 with sigma of 0.02
 O1S-C3S
 2.6 with sigma of 0.02
 O1S-C4S
 2.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C32) = Uanis(C32B)
Uanis(C33B) = Uanis(C33)
Uanis(C34B) = Uanis(C34)
Uanis(O7) = Uanis(O7B)
Uanis(O8) = Uanis(O8B)
Uanis(C1S) = Uanis(C41)
Uanis(Cl1S) = Uanis(Cl2S)
Uanis(O12B) = Uanis(O11B)
Uanis(C41) = Uanis(C40)
Uanis(C3S) = Uanis(C2S) = Uanis(C4S)
Uanis(C18) = Uanis(C18B)
Uanis(C42B) = Uanis(O11B) = Uanis(O12B)
Uanis(N4) = Uanis(C43)
Uanis(C25) = Uanis(C25B)
Uanis(Cl3S) = Uanis(S1S)
4. Rigid body (RIGU) restrains
 O11, O12, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11B, O12B, N3B, C39B, C40B, C41B, C42B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O9B, O10B, C36B, C37B, C38B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 S1S, O1S, C3S, C4S, Cl3S, C2S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11B, C42B, O12B, C41B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C43, C44, C45, O13, C46, O14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O4B)=Sof(O9B)=Sof(O10B)=Sof(H10B)=Sof(N2B)=Sof(C35B)=Sof(H35C)=Sof(H35D)=
 Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=1-FVAR(1)
 Sof(O4)=Sof(O9)=Sof(O10)=Sof(H10)=Sof(N2)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=FVAR(1)
 Sof(C18B)=1-FVAR(2)
 Sof(C18)=FVAR(2)
 Sof(H31D)=Sof(H31C)=Sof(O7B)=Sof(O8B)=Sof(H8B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=1-FVAR(3)
 Sof(H31B)=Sof(H31A)=Sof(O7)=Sof(O8)=Sof(H8)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=FVAR(3)
 Sof(S1S)=Sof(O1S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(C4S)=Sof(H4SA)=
 Sof(H4SB)=Sof(H4SC)=FVAR(4)
 Sof(C2S)=Sof(H2SB)=Sof(H2SA)=0.5*FVAR(6)
 Sof(Cl3S)=FVAR(5)
 Fixed Sof: H24(0.75) H24A(0.25) O5(0.75) O11(0.375) O12(0.375) H12A(0.375)
 N3(0.375) C25(0.75) C26(0.75) C39(0.375) H39A(0.375) H39B(0.375) C40(0.375)
 H40A(0.375) H40B(0.375) C41(0.375) H41A(0.375) H41B(0.375) C42(0.375)
 O5B(0.25) O11B(0.125) O12B(0.125) H12B(0.125) N3B(0.125) C25B(0.25) C26B(0.25)
 C39B(0.125) H39C(0.125) H39D(0.125) C40B(0.125) H40C(0.125) H40D(0.125)
 C41B(0.125) H41C(0.125) H41D(0.125) C42B(0.125) O13(0.5) O14(0.5) H14A(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) C46(0.5) Cl1S(0.125) Cl2S(0.125) C1S(0.125) H1SA(0.125) H1SB(0.125)
6.a Ternary CH refined with riding coordinates:
 C5(H5), C14(H14), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C31(H31B,H31A), C31(H31D,H31C), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C32B(H32C,H32D), C33B(H33C,H33D), C35B(H35C,H35D), C36B(H36C,
 H36D), C37B(H37C,H37D), C39B(H39C,H39D), C40B(H40C,H40D), C41B(H41C,H41D),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C1S(H1SA,H1SB), C2S(H2SB,H2SA)
6.c Me refined with riding coordinates:
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C12(H12), C16(H16), C24(H24), C24(H24A), C28(H28)
6.e Tetrahedral OH refined with riding coordinates:
 O8(H8), O10(H10), O12(H12A), O8B(H8B), O10B(H10B), O12B(H12B), O14(H14A)
;
_shelx_res_checksum              46594
_shelx_fab_checksum              6926
_olex2_submission_special_instructions 'No special instructions were received'