Polyoxovanadate-iodobodipy supramolecular assemblies: new agents for high efficiency cancer photochemotherapy.
Gu, Yaqi; Li, Qi; Huang, Yichao; Zhu, Yingting; Wei, Yongge; Ruhlmann, Laurent; Chemical communications (Cambridge, England) 56 (2020) 2869–2872; doi:10.1039/c9cc09944a

data_7125931
_publ_section_title
;
 Polyoxovanadate-iodobodipy supramolecular assemblies: new agents for high
 efficiency cancer photochemotherapy.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2869
_journal_page_last               2872
_journal_paper_doi               10.1039/c9cc09944a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'2(C24 H29 B F2 I2 N3), C10 H18 O21 V6, 2(H2 O)'
_chemical_formula_sum            'C60 H80 B2 F4 I4 N4 O23 V6'
_chemical_formula_weight         2136.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2020-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5838(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.02302(17)
_cell_length_b                   22.8571(4)
_cell_length_c                   15.9505(3)
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    109.5(7)
_cell_measurement_theta_max      74.8890
_cell_measurement_theta_min      4.7440
_cell_volume                     3652.82(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.5(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  -2.00   1.00    3.06    --  -40.81 -19.00  90.00  113
  2  \w     26.00  76.00   1.00    3.06    --   40.81-125.00 -60.00   50
  3  \w      3.00  82.00   1.00    3.06    --   40.81 -99.00 150.00   79
  4  \w     39.00 135.00   1.00   12.25    --  110.27 -30.00 120.00   96
  5  \w     84.00 111.00   1.00   12.25    --  110.27  45.00 -60.00   27
  6  \w    135.00 178.00   1.00   12.25    --  110.27  45.00 -60.00   43
  7  \w     47.00 111.00   1.00   12.25    --  110.27-125.00 -60.00   64
  8  \w     91.00 117.00   1.00   12.25    --  110.27-125.00  30.00   26
  9  \w     52.00  79.00   1.00   12.25    --  110.27-125.00  30.00   27
 10  \w     95.00 127.00   1.00   12.25    --  110.27 125.00-120.00   32
 11  \w     42.00  69.00   1.00   12.25    --  110.27 -95.00  30.00   27
 12  \w     42.00  99.00   1.00   12.25    --  110.27-125.00 150.00   57
 13  \w     30.00 105.00   1.00   12.25    --  110.27 -95.00 150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0066240000
_diffrn_orient_matrix_UB_12      -0.0669554000
_diffrn_orient_matrix_UB_13      -0.0114424000
_diffrn_orient_matrix_UB_21      -0.0728027000
_diffrn_orient_matrix_UB_22      -0.0056041000
_diffrn_orient_matrix_UB_23      0.0833718000
_diffrn_orient_matrix_UB_31      -0.1352224000
_diffrn_orient_matrix_UB_32      0.0061067000
_diffrn_orient_matrix_UB_33      -0.0473341000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15800
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.148
_diffrn_reflns_theta_min         3.868
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.589
_refine_diff_density_min         -2.353
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.633(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         10673
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                9199
_reflns_number_total             10673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09944a2.cif
_cod_data_source_block           exp_3690
_cod_depositor_comments          'Adding full bibliography for 7125931.cif.'
_cod_original_cell_volume        3652.80(12)
_cod_database_code               7125931
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'V O C N O F B I'
_shelx_estimated_absorpt_t_max   0.237
_shelx_estimated_absorpt_t_min   0.107
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.367(14)
 0.633(14)
2. 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, All O(H,H) groups
3. Restrained distances
 O21B-C49 = O21A-C49 = O20B-C58 = O20A-C58
 1.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O21A) \\sim Ueq, Uanis(O21B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O20B) \\sim Ueq, Uanis(O20A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N25) \\sim Ueq, Uanis(N32) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(N30) \\sim Ueq, Uanis(N64) \\sim Ueq, Uanis(C6) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H49A(0.6) H49B(0.6) H1(0.4) H2(0.4) O21A(0.75) H21A(0.75)
 O20B(0.5) H20B(0.5) H58A(0.5) H58B(0.5) H3(0.5) H4(0.5) O20A(0.5) H20A(0.5)
 O21B(0.25) H21B(0.25)
6.a Free rotating group:
 O23(H23A,H23B), O22(H22B,H22A)
6.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C20(H0aa,H2ba), C44(H44A,H44B), C21(H4ba,H3ba), C19(H19A,
 H19B), C43(H43A,H43B), C46(H46A,H46B), C52(H52B,H52A), C22(H1ba,H0ba),
 C54(H54B,H54A), C55(H55B,H55A), C53(H53A,H53B), C51(H50A,H50B), C49(H49A,H49B),
  C49(H1,H2), C47(H47A,H47B), C57(H57B,H57A), C23(H2aa,H3aa), C58(H58A,H58B),
 C58(H3,H4)
6.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C17(H17), C18(H18), C41(H41), C39(H39), C15(H15), C38(H38), C16(H16)
6.d Tetrahedral OH refined with riding coordinates:
 O21A(H21A), O20B(H20B), O21B(H21B)
6.e Idealised Me refined as rotating group:
 C48(H48A,H48C,H48B), C24(H24C,H24B,H24A), C12(H12C,H12B,H12A), C13(H13C,H13B,
 H13A), C36(H9aa,H7aa,H8aa), C37(H36B,H36A,H36C), C10(H10A,H10C,H10B), C11(H11C,
 H11A,H11B), C35(H35B,H35C,H35A), C34(H34C,H34B,H34A)
6.f Idealised tetrahedral OH refined as rotating group:
 O20A(H20A)
;
_olex2_date_sample_data_collection 2019-01-13
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.979
_oxdiff_exptl_absorpt_empirical_full_min 0.641