Potent Anticancer Activity with High Selectivity of a Chiral Palladium N-Heterocyclic Carbene Complex.
Kumar, Anuj; Naaz, Afsana; Prakasham, A. P.; Gangwar, Manoj Kumar; Butcher, Raymond J.; Panda, Dulal; Ghosh, Prasenjit; ACS omega 2 (2017) 4632–4646; doi:10.1021/acsomega.7b00688

data_4516899
_publ_section_title
;
 Potent Anticancer Activity with High Selectivity of a Chiral Palladium
 N-Heterocyclic Carbene Complex.
;
_journal_issue                   8
_journal_name_full               'ACS omega'
_journal_page_first              4632
_journal_page_last               4646
_journal_paper_doi               10.1021/acsomega.7b00688
_journal_volume                  2
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H50 F6 N6 O4 Pd'
_chemical_formula_sum            'C32 H50 F6 N6 O4 Pd'
_chemical_formula_weight         803.18
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-09
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.303(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.561(2)
_cell_length_b                   11.169(2)
_cell_length_c                   16.133(3)
_cell_measurement_reflns_used    6953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      4.80
_cell_volume                     1901.4(6)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_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    'Rigaku SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26732
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         29.203
_diffrn_reflns_theta_min         4.802
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.9462
_exptl_absorpt_correction_T_min  0.9109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 3574 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         10091
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0331P)^2^+0.1791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                9292
_reflns_number_total             10091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00688_si_002.cif
_cod_data_source_block           1S2S5R-1c_PG-AK-9-97
_cod_database_code               4516899
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.911
_exptl_absorpt_special_details
;
Department of Chemistry
University of Anywhere
Sometown
Somewhere, UK
;
_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.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C12(H12), C19(H19), C21(H21), C25(H25), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C17(H17A,H17B),
 C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C16(H16)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              2396
_shelx_hkl_checksum              41739
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'