Spectroscopy, electrochemistry and antiproliferative properties of Au(iii), Pt(ii) and Cu(ii) complexes bearing modified 2,2':6',2''-terpyridine ligands.
Maroń, Anna; Czerwińska, Katarzyna; Machura, Barbara; Raposo, Luis; Roma-Rodrigues, Catarina; Fernandes, Alexandra R.; Małecki, Jan G; Szlapa-Kula, Agata; Kula, Slawomir; Krompiec, Stanisław; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6444–6463; doi:10.1039/c8dt00558c

data_1549200
_publ_section_title
;
 Spectroscopy, electrochemistry and antiproliferative properties of
 Au(iii), Pt(ii) and Cu(ii) complexes bearing modified
 2,2':6',2''-terpyridine ligands.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6444
_journal_page_last               6463
_journal_paper_doi               10.1039/c8dt00558c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H20 B, C22 H17 Cl N3 O Pt, C2 H3 N'
_chemical_formula_sum            'C48 H40 B Cl N4 O Pt'
_chemical_formula_weight         930.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1mnqtt
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-12 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                77.338(3)
_cell_angle_beta                 89.736(3)
_cell_angle_gamma                76.579(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8085(3)
_cell_length_b                   15.6671(7)
_cell_length_c                   17.1368(5)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.4560
_cell_measurement_theta_min      3.7090
_cell_volume                     1987.25(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.856
_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    -63.00  -4.00   1.00   61.97    --    9.75 -57.00 -30.00   59
  2  \w     -8.00  76.00   1.00   61.97    --    9.75  38.00 -90.00   84
  3  \w     16.00  83.00   1.00   61.97    --    9.75  57.00 -60.00   67
  4  \w    -23.00  59.00   1.00   61.97    --    9.75  77.00 150.00   82
  5  \w     -2.00  47.00   1.00   61.97    --    9.75 -99.00  30.00   49
  6  \w    -70.00 -44.00   1.00   61.97    --  -11.62-179.00 -60.00   26
  7  \w    -14.00  13.00   1.00   61.97    --  -11.62  38.00-120.00   27
  8  \w    -18.00  26.00   1.00   61.97    --    9.75  57.00  90.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0302106000
_diffrn_orient_matrix_UB_12      0.0472546000
_diffrn_orient_matrix_UB_13      -0.0046670000
_diffrn_orient_matrix_UB_21      0.0068780000
_diffrn_orient_matrix_UB_22      0.0059212000
_diffrn_orient_matrix_UB_23      -0.0420370000
_diffrn_orient_matrix_UB_31      -0.0882241000
_diffrn_orient_matrix_UB_32      -0.0037156000
_diffrn_orient_matrix_UB_33      -0.0038775000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23654
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.508
_diffrn_reflns_theta_min         3.354
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.640
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.555
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.965
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0528P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7353
_reflns_number_total             9487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00558c2.cif
_cod_data_source_block           ptdmsoewm20pf6a
_cod_depositor_comments
'Adding full bibliography for 1549200--1549203.cif.'
_cod_original_cell_volume        1987.24(14)
_cod_database_code               1549200
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Pt1 N4 O1 Cl1 B1 C48 H40'
_reflns_odcompleteness_completeness 99.78
_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
2. Others
 Sof(H44)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C45A)=Sof(H45A)=
 Sof(C46A)=Sof(H46A)=1-FVAR(1)
 Sof(H44A)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=Sof(C45)=Sof(H45)=Sof(C46)=
 Sof(H46)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C44(H44), C44(H44A), C42A(H42A), C43A(H43A), C45A(H45A), C46A(H46A), C42(H42),
  C43(H43), C45(H45), C46(H46), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9),
 C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20),
  C21(H21)
3.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              70629
_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 2.122
_oxdiff_exptl_absorpt_empirical_full_min 0.656