#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313530.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313530
loop_
_publ_author_name
'David Amantia'
'Clayton Price'
'Michelle A. Shipman'
'Mark R. J. Elsegood'
'William Clegg'
'Andrew Houlton'
_publ_section_title
;
 Minor Groove Site Coordination of Adenine by Platinum Group Metal Ions:
 Effects on Basicity, Base Pairing, and Electronic Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3047
_journal_page_last               3056
_journal_paper_doi               10.1021/ic020657g
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H16 B Cl F4 N5 O0.5 Pd S2'
_chemical_formula_weight         507.06
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.116(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.3530(11)
_cell_length_b                   30.641(3)
_cell_length_c                   8.5451(7)
_cell_measurement_reflns_used    14196
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.73
_cell_volume                     3496.2(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25301
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00008(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         8316
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                6806
_reflns_number_total             8316
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020657g_2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C10 H16 B Cl F4 N5 O0.50 Pd S2'
_cod_database_code               4313530
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.08764(3) 0.871437(10) 0.64633(5) 0.01531(8) Uani 1 1 d . . .
Cl1 Cl 1.14044(9) 0.91272(4) 0.43567(13) 0.0237(3) Uani 1 1 d . . .
N1 N 0.8479(3) 0.96501(11) 0.6443(5) 0.0168(8) Uani 1 1 d . . .
C2 C 0.9207(4) 0.93680(15) 0.6151(5) 0.0178(10) Uani 1 1 d . . .
H2 H 0.9269 0.9278 0.5091 0.021 Uiso 1 1 calc R . .
N3 N 0.9873(3) 0.91910(13) 0.7158(4) 0.0171(9) Uani 1 1 d . . .
C4 C 0.9732(3) 0.93321(13) 0.8675(6) 0.0140(9) Uani 1 1 d . . .
C5 C 0.8984(4) 0.96080(14) 0.9136(5) 0.0144(9) Uani 1 1 d . . .
C6 C 0.8324(4) 0.97797(14) 0.7973(5) 0.0153(10) Uani 1 1 d . . .
N6 N 0.7604(3) 1.00662(12) 0.8259(4) 0.0197(9) Uani 1 1 d . . .
H6A H 0.7239 1.0169 0.7484 0.024 Uiso 1 1 calc R . .
H6B H 0.7492 1.0154 0.9224 0.024 Uiso 1 1 calc R . .
N7 N 0.9044(3) 0.96890(12) 1.0731(4) 0.0187(9) Uani 1 1 d . . .
C8 C 0.9824(4) 0.94523(15) 1.1182(5) 0.0223(11) Uani 1 1 d . . .
H8 H 1.0049 0.9440 1.2237 0.027 Uiso 1 1 calc R . .
N9 N 1.0278(3) 0.92264(13) 0.9986(4) 0.0178(9) Uani 1 1 d . . .
C10 C 1.1196(4) 0.89663(15) 1.0150(5) 0.0192(11) Uani 1 1 d . . .
H10A H 1.1549 0.9057 1.1117 0.023 Uiso 1 1 calc R . .
H10B H 1.1642 0.9029 0.9254 0.023 Uiso 1 1 calc R . .
C11 C 1.1002(4) 0.84768(16) 1.0219(5) 0.0238(11) Uani 1 1 d . . .
H11A H 1.0599 0.8409 1.1161 0.029 Uiso 1 1 calc R . .
H11B H 1.1648 0.8321 1.0315 0.029 Uiso 1 1 calc R . .
S12 S 1.03315(9) 0.82785(4) 0.84613(17) 0.0229(3) Uani 1 1 d . . .
C13 C 1.0967(4) 0.77643(15) 0.8077(6) 0.0299(13) Uani 1 1 d . . .
H13A H 1.1005 0.7593 0.9057 0.036 Uiso 1 1 calc R . .
H13B H 1.0573 0.7594 0.7307 0.036 Uiso 1 1 calc R . .
C14 C 1.2015(5) 0.78354(17) 0.7449(6) 0.0322(14) Uani 1 1 d . . .
H14A H 1.2327 0.7551 0.7192 0.039 Uiso 1 1 calc R . .
H14B H 1.2434 0.7982 0.8248 0.039 Uiso 1 1 calc R . .
S15 S 1.19300(10) 0.81738(4) 0.56949(16) 0.0239(3) Uani 1 1 d . . .
C16 C 1.3192(4) 0.83881(19) 0.5620(7) 0.0372(14) Uani 1 1 d . . .
H16A H 1.3350 0.8533 0.6612 0.056 Uiso 1 1 calc R . .
H16B H 1.3244 0.8599 0.4761 0.056 Uiso 1 1 calc R . .
H16C H 1.3664 0.8148 0.5445 0.056 Uiso 1 1 calc R . .
Pd1A Pd 0.61055(3) 0.890210(10) 0.85261(5) 0.01531(8) Uani 1 1 d . . .
Cl1A Cl 0.63888(10) 0.93419(4) 1.06844(14) 0.0231(3) Uani 1 1 d . . .
N1A N 0.3270(3) 0.95816(11) 0.8559(5) 0.0172(8) Uani 1 1 d . . .
C2A C 0.4131(4) 0.93706(14) 0.8868(5) 0.0174(10) Uani 1 1 d . . .
H2A H 0.4240 0.9290 0.9928 0.021 Uiso 1 1 calc R . .
N3A N 0.4855(3) 0.92605(12) 0.7854(4) 0.0161(9) Uani 1 1 d . . .
C4A C 0.4645(3) 0.93844(13) 0.6342(6) 0.0133(9) Uani 1 1 d . . .
C5A C 0.3785(4) 0.96002(14) 0.5892(5) 0.0148(10) Uani 1 1 d . . .
C6A C 0.3071(4) 0.97154(14) 0.7048(5) 0.0148(10) Uani 1 1 d . . .
N6A N 0.2252(3) 0.99465(12) 0.6766(4) 0.0209(9) Uani 1 1 d . . .
H6A1 H 0.1843 1.0013 0.7537 0.025 Uiso 1 1 calc R . .
H6A2 H 0.2116 1.0034 0.5808 0.025 Uiso 1 1 calc R . .
N7A N 0.3804(3) 0.96887(12) 0.4278(5) 0.0176(9) Uani 1 1 d . . .
C8A C 0.4663(4) 0.95258(15) 0.3836(5) 0.0186(11) Uani 1 1 d . . .
H8A H 0.4890 0.9537 0.2783 0.022 Uiso 1 1 calc R . .
N9A N 0.5215(3) 0.93353(13) 0.5031(4) 0.0161(9) Uani 1 1 d . . .
C10A C 0.6238(4) 0.91664(16) 0.4867(5) 0.0236(12) Uani 1 1 d . . .
H10C H 0.6644 0.9266 0.5771 0.028 Uiso 1 1 calc R . .
H10D H 0.6541 0.9290 0.3907 0.028 Uiso 1 1 calc R . .
C11A C 0.6279(4) 0.86634(16) 0.4778(6) 0.0254(12) Uani 1 1 d . . .
H11C H 0.6981 0.8569 0.4628 0.030 Uiso 1 1 calc R . .
H11D H 0.5884 0.8562 0.3867 0.030 Uiso 1 1 calc R . .
S12A S 0.57798(9) 0.84162(4) 0.65679(16) 0.0211(2) Uani 1 1 d . . .
C13A C 0.6683(4) 0.79784(15) 0.6939(6) 0.0251(12) Uani 1 1 d . . .
H13C H 0.6405 0.7775 0.7726 0.030 Uiso 1 1 calc R . .
H13D H 0.6796 0.7813 0.5960 0.030 Uiso 1 1 calc R . .
C14A C 0.7672(4) 0.81562(17) 0.7524(6) 0.0264(12) Uani 1 1 d . . .
H14C H 0.8016 0.8307 0.6652 0.032 Uiso 1 1 calc R . .
H14D H 0.8101 0.7910 0.7859 0.032 Uiso 1 1 calc R . .
S15A S 0.75363(9) 0.85354(4) 0.91539(14) 0.0211(3) Uani 1 1 d . . .
C16A C 0.7148(5) 0.81664(19) 1.0691(6) 0.0387(15) Uani 1 1 d . . .
H16D H 0.6534 0.8015 1.0370 0.058 Uiso 1 1 calc R . .
H16E H 0.7021 0.8332 1.1650 0.058 Uiso 1 1 calc R . .
H16F H 0.7678 0.7952 1.0884 0.058 Uiso 1 1 calc R . .
B1 B 0.3900(6) 0.8302(2) 0.1063(8) 0.0578(18) Uani 1 1 d DU . .
F1 F 0.3326(15) 0.7957(6) 0.128(2) 0.132(7) Uani 0.488(12) 1 d PDU A 1
F2 F 0.4755(8) 0.8277(6) 0.1887(17) 0.112(5) Uani 0.488(12) 1 d PDU A 1
F3 F 0.3428(13) 0.8677(4) 0.1519(19) 0.133(6) Uani 0.488(12) 1 d PDU A 1
F4 F 0.4186(16) 0.8292(5) -0.0429(12) 0.124(6) Uani 0.488(12) 1 d PDU A 1
F1X F 0.3223(15) 0.8082(6) 0.1879(18) 0.129(6) Uani 0.512(12) 1 d PDU A 2
F2X F 0.4658(12) 0.8020(6) 0.074(3) 0.226(8) Uani 0.512(12) 1 d PDU A 2
F3X F 0.4348(12) 0.8608(4) 0.1925(11) 0.112(6) Uani 0.512(12) 1 d PDU A 2
F4X F 0.3500(10) 0.8445(4) -0.0278(12) 0.085(4) Uani 0.512(12) 1 d PDU A 2
B2 B 0.8950(5) 0.8059(2) 0.3869(7) 0.0290(14) Uani 1 1 d . . .
F5 F 0.9380(3) 0.80011(12) 0.2410(4) 0.0442(10) Uani 1 1 d . . .
F6 F 0.8761(3) 0.85021(10) 0.4121(5) 0.0515(10) Uani 1 1 d . . .
F7 F 0.8061(2) 0.78310(10) 0.3955(3) 0.0357(8) Uani 1 1 d . . .
F8 F 0.9600(3) 0.79120(13) 0.5049(4) 0.0473(9) Uani 1 1 d . . .
O1W O 0.5115(4) 0.7627(2) 0.4093(7) 0.095(2) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 N3 92.06(11) . . ?
Cl1 Pd1 S12 177.11(5) . . ?
Cl1 Pd1 S15 89.07(5) . . ?
N3 Pd1 S12 89.47(11) . . ?
N3 Pd1 S15 177.90(12) . . ?
S12 Pd1 S15 89.32(5) . . ?
C2 N1 C6 118.5(4) . . ?
N1 C2 N3 128.7(4) . . ?
Pd1 N3 C2 121.8(3) . . ?
Pd1 N3 C4 125.5(3) . . ?
C2 N3 C4 112.5(4) . . ?
N3 C4 C5 124.4(4) . . ?
N3 C4 N9 128.2(4) . . ?
C5 C4 N9 107.3(4) . . ?
C4 C5 C6 118.5(4) . . ?
C4 C5 N7 110.6(4) . . ?
C6 C5 N7 130.7(4) . . ?
N1 C6 C5 117.3(4) . . ?
N1 C6 N6 118.4(4) . . ?
C5 C6 N6 124.3(4) . . ?
C5 N7 C8 103.4(4) . . ?
N7 C8 N9 114.0(4) . . ?
C4 N9 C8 104.6(4) . . ?
C4 N9 C10 130.3(4) . . ?
C8 N9 C10 124.8(4) . . ?
N9 C10 C11 113.4(4) . . ?
C10 C11 S12 112.0(3) . . ?
Pd1 S12 C11 105.09(16) . . ?
Pd1 S12 C13 102.81(18) . . ?
C11 S12 C13 101.9(2) . . ?
S12 C13 C14 111.8(4) . . ?
C13 C14 S15 108.4(4) . . ?
Pd1 S15 C14 102.38(19) . . ?
Pd1 S15 C16 108.85(19) . . ?
C14 S15 C16 100.3(3) . . ?
Cl1A Pd1A N3A 92.44(11) . . ?
Cl1A Pd1A S12A 174.35(5) . . ?
Cl1A Pd1A S15A 87.93(5) . . ?
N3A Pd1A S12A 89.44(11) . . ?
N3A Pd1A S15A 176.30(11) . . ?
S12A Pd1A S15A 90.54(5) . . ?
C2A N1A C6A 119.3(4) . . ?
N1A C2A N3A 127.6(4) . . ?
Pd1A N3A C2A 122.2(3) . . ?
Pd1A N3A C4A 124.6(3) . . ?
C2A N3A C4A 113.0(4) . . ?
N3A C4A C5A 124.2(4) . . ?
N3A C4A N9A 128.9(4) . . ?
C5A C4A N9A 106.8(4) . . ?
C4A C5A C6A 119.1(4) . . ?
C4A C5A N7A 110.4(4) . . ?
C6A C5A N7A 130.4(4) . . ?
N1A C6A C5A 116.6(4) . . ?
N1A C6A N6A 119.1(4) . . ?
C5A C6A N6A 124.2(4) . . ?
C5A N7A C8A 103.2(4) . . ?
N7A C8A N9A 114.4(4) . . ?
C4A N9A C8A 105.2(4) . . ?
C4A N9A C10A 129.6(4) . . ?
C8A N9A C10A 124.9(4) . . ?
N9A C10A C11A 112.9(4) . . ?
C10A C11A S12A 111.0(3) . . ?
Pd1A S12A C11A 105.85(17) . . ?
Pd1A S12A C13A 103.10(17) . . ?
C11A S12A C13A 101.9(2) . . ?
S12A C13A C14A 111.6(3) . . ?
C13A C14A S15A 113.2(4) . . ?
Pd1A S15A C14A 102.65(17) . . ?
Pd1A S15A C16A 103.7(2) . . ?
C14A S15A C16A 100.7(3) . . ?
F1 B1 F2 111.9(12) . . ?
F1 B1 F3 111.4(13) . . ?
F1 B1 F4 106.7(11) . . ?
F2 B1 F3 106.9(10) . . ?
F2 B1 F4 104.8(12) . . ?
F3 B1 F4 115.1(11) . . ?
F1X B1 F2X 106.9(13) . . ?
F1X B1 F3X 111.9(10) . . ?
F1X B1 F4X 110.3(11) . . ?
F2X B1 F3X 103.0(11) . . ?
F2X B1 F4X 109.3(12) . . ?
F3X B1 F4X 114.9(9) . . ?
F5 B2 F6 109.8(5) . . ?
F5 B2 F7 110.0(5) . . ?
F5 B2 F8 110.4(5) . . ?
F6 B2 F7 109.2(5) . . ?
F6 B2 F8 108.2(5) . . ?
F7 B2 F8 109.2(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.3114(13) . ?
Pd1 N3 2.070(4) . ?
Pd1 S12 2.2875(14) . ?
Pd1 S15 2.2710(13) . ?
N1 C2 1.325(6) . ?
N1 C6 1.383(6) . ?
C2 N3 1.350(6) . ?
N3 C4 1.379(6) . ?
C4 C5 1.367(6) . ?
C4 N9 1.374(6) . ?
C5 C6 1.428(6) . ?
C5 N7 1.388(5) . ?
C6 N6 1.324(6) . ?
N7 C8 1.325(6) . ?
C8 N9 1.377(6) . ?
N9 C10 1.468(6) . ?
C10 C11 1.523(7) . ?
C11 S12 1.849(5) . ?
S12 C13 1.820(5) . ?
C13 C14 1.516(8) . ?
C14 S15 1.826(5) . ?
S15 C16 1.809(6) . ?
Pd1A Cl1A 2.3147(12) . ?
Pd1A N3A 2.078(4) . ?
Pd1A S12A 2.2809(13) . ?
Pd1A S15A 2.2794(13) . ?
N1A C2A 1.345(6) . ?
N1A C6A 1.380(6) . ?
C2A N3A 1.343(6) . ?
N3A C4A 1.375(6) . ?
C4A C5A 1.379(6) . ?
C4A N9A 1.364(6) . ?
C5A C6A 1.419(6) . ?
C5A N7A 1.406(6) . ?
C6A N6A 1.325(6) . ?
N7A C8A 1.307(6) . ?
C8A N9A 1.387(6) . ?
N9A C10A 1.468(6) . ?
C10A C11A 1.544(7) . ?
C11A S12A 1.833(5) . ?
S12A C13A 1.832(5) . ?
C13A C14A 1.512(7) . ?
C14A S15A 1.823(5) . ?
S15A C16A 1.810(6) . ?
B1 F1 1.320(10) . ?
B1 F2 1.343(10) . ?
B1 F3 1.367(10) . ?
B1 F4 1.332(10) . ?
B1 F1X 1.327(11) . ?
B1 F2X 1.361(11) . ?
B1 F3X 1.334(9) . ?
B1 F4X 1.337(9) . ?
B2 F5 1.385(7) . ?
B2 F6 1.397(7) . ?
B2 F7 1.380(7) . ?
B2 F8 1.403(7) . ?
