Investigation of cobalt(III)-tpa complexes as potential bioreductively activated carriers for naphthoquinone-based drugs
Lanznaster, Mauricio; da Silva, Aline Farias Moreira; Vital, Renata de Uzeda; Martins, Daniela de Luna; Rocha, David Rodrigues; Ferreira, Glaucio Braga; Camargos-Resende, Jackson A. L.; New J. Chem. 41 (2017) 14960–14965; doi:10.1039/C7NJ03072J

data_7056721
_publ_section_title
;
 Investigation of cobalt(III)-tpa complexes as potential bioreductively
 activated carriers for naphthoquinone-based drugs
;
_journal_issue                   24
_journal_name_full               'New J. Chem.'
_journal_page_first              14960
_journal_page_last               14965
_journal_paper_doi               10.1039/C7NJ03072J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C29 H25 Br Co N4 O4, B F4, 1(H2 O)'
_chemical_formula_sum            'C29 H27 B Br Co F4 N4 O5'
_chemical_formula_weight         737.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 93.9895(13)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.23899(16)
_cell_length_b                   8.76417(12)
_cell_length_c                   33.1396(4)
_cell_measurement_reflns_used    43160
_cell_measurement_temperature    149.8(2)
_cell_measurement_theta_max      29.8290
_cell_measurement_theta_min      1.8443
_cell_volume                     2966.62(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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_temperature      150.15
_diffrn_detector_area_resol_mean 10.4186
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -69.00    2.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -      -10.6780  126.0000  144.0000 71

  2 omega  -15.00   87.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   57.0000   60.0000 102

  3 omega  -66.00   47.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -77.0000   60.0000 113

  4 omega  -20.00   67.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   77.0000 -180.0000 87

  5 omega  -65.00   46.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -77.0000  -60.0000 111

  6 omega  -14.00   89.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   38.0000    0.0000 103

  7 omega    8.00   53.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -91.0000  101.0000 45

  8 omega  -87.00   16.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -      -10.6780  -38.0000 -180.0000 103

  9 omega -100.00  -34.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -      -10.6780 -179.0000 -150.0000 66

 10 omega -100.00  -32.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -      -10.6780  179.0000   30.0000 68

 11 omega  -21.00   92.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   77.0000  120.0000 113

 12 omega   19.00   71.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655 -126.0000   35.0000 52

 13 omega  -17.00   87.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   57.0000  -30.0000 104

 14 omega  -61.00   42.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -57.0000 -150.0000 103

 15 omega   -4.00   55.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -99.0000  -60.0000 59

 16 omega   -4.00   55.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -99.0000  150.0000 59

 17 omega  -14.00   89.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655   38.0000   30.0000 103

 18 omega   19.00   71.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655 -126.0000 -112.0000 52

 19 omega  -13.00   53.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       14.0000  -91.0000  101.0000 66

 20 omega  -88.00  -15.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -      -10.6780  154.0000 -143.0000 73

 21 omega   -4.00   55.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -99.0000  -90.0000 59

 22 omega   -4.00   55.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -99.0000 -180.0000 59

 23 omega  -77.00  102.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655    0.0000 -180.0000 179

 24 omega  -77.00   98.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655    0.0000 -150.0000 175

 25 omega  -63.00   39.00   1.0000   13.7100
omega____ theta____ kappa____ phi______ frames
    -       12.8655  -38.0000  -60.0000 102
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0650739000
_diffrn_orient_matrix_UB_12      -0.0043421000
_diffrn_orient_matrix_UB_13      0.0059927000
_diffrn_orient_matrix_UB_21      -0.0235916000
_diffrn_orient_matrix_UB_22      -0.0073873000
_diffrn_orient_matrix_UB_23      -0.0205472000
_diffrn_orient_matrix_UB_31      0.0056500000
_diffrn_orient_matrix_UB_32      -0.0804525000
_diffrn_orient_matrix_UB_33      0.0015581000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            149913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.80185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0347P)^2^+7.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5083
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03072j2.cif
_cod_data_source_block           colaubhtpa-agua
_cod_original_cell_volume        2966.61(8)
_cod_database_code               7056721
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Co C28 H22 N4 O3 B2 F8 Br '
_cell_oxdiff_angle_alpha         90.0121(12)
_cell_oxdiff_angle_beta          93.9852(13)
_cell_oxdiff_angle_gamma         90.0224(13)
_cell_oxdiff_length_a            10.23807(18)
_cell_oxdiff_length_b            8.76679(13)
_cell_oxdiff_length_c            33.1325(5)
_cell_oxdiff_measurement_reflns_used 43160
_cell_oxdiff_volume              2966.61(8)
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.559
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 O2W, O1W, O3W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F21, F11, F22, F12, B1, F23, F13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 1*[Sof(O2W)+Sof(H2WA)+Sof(H2WB)]+1*[Sof(O3W)+Sof(H3WA)+Sof(H3WB)]+1*[Sof(O1W)+
 Sof(H1WA)+Sof(H1WB)]=1 with esd of 0.001
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(1)
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=FVAR(2)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F21)=1-FVAR(4)
 Sof(F13)=Sof(F12)=Sof(F11)=FVAR(4)
4.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C36(H36A,H36B), C46(H46A,H46B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C21(H21), C22(H22), C23(H23), C24(H24),
 C31(H31), C32(H32), C33(H33), C34(H34), C41(H41), C42(H42), C44(H44), C43(H43)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              15381
_olex2_submission_special_instructions 'No special instructions were received'