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_4516900
_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         'C42 H54 F6 N6 O4 Pd'
_chemical_formula_sum            'C42 H54 F6 N6 O4 Pd'
_chemical_formula_weight         927.31
_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             2017-07-11
_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                 109.578(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.702(3)
_cell_length_b                   20.111(6)
_cell_length_c                   11.874(4)
_cell_measurement_reflns_used    5437
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      4.63
_cell_volume                     2182.9(12)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1012
_diffrn_reflns_av_unetI/netI     0.2040
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13887
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         4.627
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 1241 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7334
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                4673
_reflns_number_total             7334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00688_si_002.cif
_cod_data_source_block           1S2S5R-3c_PG-AK-9-85
_cod_database_code               4516900
_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. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of
-0.1 and sigma for terminal atoms of -0.2
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C14(H14), C16(H16), C30(H30), C31(H31), C34(H34), C35(H35)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C22(H22A,H22B),
 C29(H29A,H29B), C32(H32A,H32B), C33(H33A,H33B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C21(H21), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              80251
_shelx_hkl_checksum              48946
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'