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_4516896
_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         'C38 H54 Br2 N6 Pd'
_chemical_formula_sum            'C38 H54 Br2 N6 Pd'
_chemical_formula_weight         861.09
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 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-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                98.396(4)
_cell_angle_beta                 95.925(4)
_cell_angle_gamma                101.192(3)
_cell_formula_units_Z            2
_cell_length_a                   11.565(3)
_cell_length_b                   13.039(3)
_cell_length_c                   13.719(3)
_cell_measurement_reflns_used    13098
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.02
_cell_volume                     1989.1(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_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    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35247
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.625
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 4079 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         12811
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0458P)^2^+0.6592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.894
_reflns_Friedel_fraction_max     0.894
_reflns_number_gt                10780
_reflns_number_total             12811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00688_si_002.cif
_cod_data_source_block           1R2R5S-3b_PG-AK-11-223
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H108 Br4 N12 Pd2'
_cod_original_formula_weight         1722.18
_cod_original_formula_moiety         '2(C38 H54 Br2 N6 Pd)'
_cod_original_formula_units_Z            1
_cod_database_code               4516896
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.457
_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(N10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of -0.1 and sigma for
terminal atoms of -0.2
Uanis(C51) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C59) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of -0.1 and sigma for
terminal atoms of -0.2
Uanis(C9) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of -0.1 and sigma for
terminal atoms of -0.2
Uanis(C12) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of
-0.1 and sigma for terminal atoms of -0.2
Uanis(C45) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of -0.1 and sigma for
terminal atoms of -0.2
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C23(H23), C25(H25), C29(H29), C30(H30), C33(H33), C35(H35), C39(H39),
 C40(H40), C57(H57), C59(H59), C63(H63), C64(H64), C67(H67), C69(H69), C73(H73),
  C74(H74)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C16(H16A,H16B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B),
 C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B), C43(H43A,H43B), C50(H50A,H50B),
  C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C68(H68A,H68B), C71(H71A,
 H71B), C72(H72A,H72B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C7(H7), C8(H8), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
3.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C36(H36A,H36B,
 H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C60(H60A,H60B,H60C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'