A binuclear Fe(iii)/quinizarin complex as a structural model for anthracycline drugs binding to iron
do Nascimento, Juliana S.; de Sousa, Aurideia P.; Gondim, Ana C. S.; Sousa, Eduardo H. S.; Teixeira, Edson H.; do Nascimento Neto, Luiz Gonzaga; Bezerra, Beatriz Pinheiro; Ayala, Alejandro Pedro; Batista, Alzir A.; Vasconcelos, Igor F.; Oliveira, Francisco G. S.; Holanda, Alda K. M.; New Journal of Chemistry 46 (2022) 5515–5525; doi:10.1039/D1NJ04087A

data_7061319
_publ_section_title
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 A binuclear Fe(iii)/quinizarin complex as a structural model for
 anthracycline drugs binding to iron
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5515
_journal_page_last               5525
_journal_paper_doi               10.1039/D1NJ04087A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C34 H54 Fe2 N8 O4, Cl, 3(F6 P)'
_chemical_formula_sum            'C34 H54 Cl F18 Fe2 N8 O4 P3'
_chemical_formula_weight         1220.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.069(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0603(5)
_cell_length_b                   16.6212(6)
_cell_length_c                   17.6984(7)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      71.39
_cell_measurement_theta_min      2.75
_cell_volume                     4721.4(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CPAD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            63999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.467
_diffrn_reflns_theta_min         3.649
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.501
_exptl_absorpt_correction_T_max  0.7104
_exptl_absorpt_correction_T_min  0.4063
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.5719.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull brownish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       plate
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         8661
_refine_ls_number_restraints     624
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0856
_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^)+(0.1526P)^2^+4.6539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2318
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5085
_reflns_number_total             8661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04087a2.cif
_cod_data_source_block           cu_binuclear
_cod_depositor_comments          'Adding full bibliography for 7061319.cif.'
_cod_database_code               7061319
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
P1A \\sim F1A \\sim F2A \\sim F3A' \\sim F4A \\sim F5A \\sim F6A \\sim F1A'
\\sim F2A' \\sim F3A \\sim F4A' \\sim F5A' \\sim F6A': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
P1B \\sim F1B \\sim F2B \\sim F3B \\sim F4B \\sim F5B \\sim F6B \\sim F1B'
\\sim F2B' \\sim F3B' \\sim F4B' \\sim F5B' \\sim F6B': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
P1C \\sim F1C \\sim F2C \\sim F3C \\sim F4C \\sim F5C \\sim F6C \\sim F1C'
\\sim F2C' \\sim F3C' \\sim F4C' \\sim F5C' \\sim F6C': within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C6B) = Uanis(C7B)
Uanis(C9B) = Uanis(C10B)
3. Rigid body (RIGU) restrains
 N1B, N5B, N8B, N12B, C2B, C3B, C4B, C6B, C7B, C9B, C10B, C11B, C13B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5A, C6A, C7A, N8A, C9A, C10A, N11A, C12A, C13A, C14A, N1A, C2A, C3A, N4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F1A(0.5) F2A(0.5) F3A'(0.5) F4A(0.5) F5A(0.5) F6A(0.5) F1A'(0.5)
 F2A'(0.5) F3A(0.5) F4A'(0.5) F5A'(0.5) F6A'(0.5) F1B(0.5) F2B(0.5) F3B(0.5)
 F4B(0.5) F5B(0.5) F6B(0.5) F1B'(0.5) F2B'(0.5) F3B'(0.5) F4B'(0.5) F5B'(0.5)
 F6B'(0.5) F1C(0.5) F2C(0.5) F3C(0.5) F4C(0.5) F5C(0.5) F6C(0.5) F1C'(0.5)
 F2C'(0.5) F3C'(0.5) F4C'(0.5) F5C'(0.5) F6C'(0.5)
5.a Ternary CH refined with riding coordinates:
 N1A(H1A), N1B(H1B), N4A(H4A), N5B(H5B), N8A(H8A), N8B(H8B), N11A(H11A),
 N12B(H12B)
5.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4B(H4BA,
 H4BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7A(H7AA,H7AB),
 C7B(H7BA,H7BB), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C10A(H10A,H10B), C10B(H10C,
 H10D), C11B(H11B,H11C), C12A(H12A,H12C), C13A(H13A,H13B), C13B(H13C,H13D),
 C14A(H14A,H14B), C14B(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16)
;
_shelx_res_checksum              11146
_olex2_submission_special_instructions 'No special instructions were received'