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_4516897
_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             2017-07-12
_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                 95.294(4)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   18.899(5)
_cell_length_b                   11.212(3)
_cell_length_c                   27.511(7)
_cell_measurement_reflns_used    18768
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.02
_cell_volume                     5805(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0985
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            67066
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.070
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 4302 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1348
_refine_ls_number_reflns         18758
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0435P)^2^+13.7358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                15902
_reflns_number_total             18758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b00688_si_002.cif
_cod_data_source_block           1R2R5S-1c_PG-AK-11-225
_cod_depositor_comments
;

2020-07-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H150 F18 N18 O12 Pd3'
_cod_original_formula_weight         2409.53
_cod_original_formula_moiety         '3(C32 H50 F6 N6 O4 Pd)'
_cod_original_formula_units_Z            2
_cod_database_code               4516897
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.932
_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(C9) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
-0.1 and sigma for terminal atoms of -0.2
Uanis(F6) \\sim Ueq, Uanis(F3AA) \\sim Ueq, Uanis(F2AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C13(H13), C15(H15), C19(H19), C20(H20), C25(H25), C27(H27), C31(H31),
 C32(H32), C37(H37), C39(H39), C43(H43), C44(H44), C49(H49), C51(H51), C55(H55),
  C56(H56), C61(H61), C63(H63), C67(H67), C68(H68), C73(H73), C75(H75),
 C79(H79), C80(H80)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B), C23(H23A,H23B), C26(H26A,
 H26B), C29(H29A,H29B), C30(H30A,H30B), C35(H35A,H35B), C38(H38A,H38B),
 C41(H41A,H41B), C42(H42A,H42B), C47(H47A,H47B), C50(H50A,H50B), C53(H53A,H53B),
  C54(H54A,H54B), C59(H59A,H59B), C62(H62A,H62B), C65(H65A,H65B), C66(H66A,
 H66B), C71(H71A,H71B), C74(H74A,H74B), C77(H77A,H77B), C78(H78A,H78B),
 C83(H83A,H83B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C84(H84A,H84B,H84C)
;
_shelx_res_checksum              15815
_shelx_hkl_checksum              73840
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'