Mn(III), Zn(II) and Pt(II) macroacyclic complexes: Synthesis, X-ray structures, anticancer and antioxidant activities
Keypour, Hassan; Ansari, Neda; Mahmoudabadi, Masoumeh; Karamian, Roya; Moazzami Farida, Seyed Hamed; Eslami Moghadam, Mahboube; William Gable, Robert; Inorganica Chimica Acta 509 (2020) 119705–; doi:10.1016/j.ica.2020.119705

data_1564473
_publ_section_title
;
 Mn(III), Zn(II) and Pt(II) macroacyclic complexes: Synthesis, X-ray
 structures, anticancer and antioxidant activities
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119705
_journal_paper_doi               10.1016/j.ica.2020.119705
_journal_volume                  509
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C18 H24 N4 Pt, 0.292(I), 1.708(Cl), 0.727(H2 O)'
_chemical_formula_sum            'C18 H25.45 Cl1.708 I0.292 N4 O0.727 Pt'
_chemical_formula_weight         602.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 105.741(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1878(3)
_cell_length_b                   27.6088(10)
_cell_length_c                   9.0472(3)
_cell_measurement_reflns_used    5397
_cell_measurement_temperature    100.2(3)
_cell_measurement_theta_max      32.0990
_cell_measurement_theta_min      3.7310
_cell_volume                     1968.47(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_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     -5.00  85.00   1.00   12.00    --   17.98  57.00   0.00   90
  2  \w    -53.00  41.00   1.00   12.00    --   17.98 -57.00-150.00   94
  3  \w    -88.00   9.00   1.00   12.00    --  -18.60 -77.00  90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0017272000
_diffrn_orient_matrix_UB_12      0.0157053000
_diffrn_orient_matrix_UB_13      0.0624524000
_diffrn_orient_matrix_UB_21      -0.0428014000
_diffrn_orient_matrix_UB_22      0.0180229000
_diffrn_orient_matrix_UB_23      -0.0521087000
_diffrn_orient_matrix_UB_31      -0.0791377000
_diffrn_orient_matrix_UB_32      -0.0094006000
_diffrn_orient_matrix_UB_33      0.0044961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8604
_diffrn_reflns_point_group_measured_fraction_full 0.852
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.198
_diffrn_reflns_theta_min         2.688
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       plate
_exptl_crystal_F_000             1159
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation from ethanol'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.054(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4875
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.539
_reflns_Friedel_fraction_full    0.704
_reflns_Friedel_fraction_max     0.491
_reflns_number_gt                4769
_reflns_number_total             4875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rwg2019_17bGau.cif
_cod_data_source_block           rwg2019_17bgau
_cod_original_cell_volume        1968.48(13)
_cod_database_code               1564473
_chemical_oxdiff_formula         'C18 H25.6 Cl1.7 I0.3 N4 O0.7 Pt'
_chemical_oxdiff_usercomment     MAH2
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.946(7)
 0.054(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(I1)
Uanis(Cl2) = Uanis(I2)
4. Others
 Sof(I2)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(I1)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Sof(O1)=Sof(H1C)=Sof(H1D)=FVAR(3)
5.a Free rotating group:
 O1(H1C,H1D)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17)
;
_shelx_res_checksum              63787
_shelx_hkl_checksum              29816
_olex2_exptl_crystal_mounting_method 'mounted on a cryoloop'
_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 1.554
_oxdiff_exptl_absorpt_empirical_full_min 0.794