#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313534.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_4313534
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            'C16 H29 Cl3 N7 O2 Rh S2'
_chemical_formula_weight         624.84
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.213(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9976(9)
_cell_length_b                   8.6960(5)
_cell_length_c                   18.8943(11)
_cell_measurement_reflns_used    17127
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.23
_cell_volume                     2482.1(2)
_computing_cell_refinement       'Bruker SAINT'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16939
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.776
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0221P)²+7.1669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                3944
_reflns_number_total             4364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020657g_6.cif
_cod_data_source_block           5
_cod_database_code               4313534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Rh1 Rh 0.124383(17) 0.20216(3) 0.409864(16) 0.01364(9) Uani 1 1 d . . .
Cl1 Cl 0.21803(6) 0.07082(10) 0.35678(5) 0.0237(2) Uani 1 1 d . . .
Cl2 Cl 0.11541(6) 0.40142(10) 0.32218(5) 0.0232(2) Uani 1 1 d . . .
Cl3 Cl 0.03723(6) 0.34701(10) 0.46301(5) 0.0234(2) Uani 1 1 d . . .
N1 N -0.14590(19) 0.1587(3) 0.27000(17) 0.0180(6) Uani 1 1 d . . .
C2 C -0.0611(2) 0.1913(4) 0.3037(2) 0.0182(7) Uani 1 1 d . . .
H2 H -0.0450 0.2958 0.3013 0.022 Uiso 1 1 calc R . .
N3 N 0.00535(18) 0.0963(3) 0.34104(16) 0.0152(6) Uani 1 1 d . . .
C4 C -0.0222(2) -0.0522(4) 0.34079(18) 0.0140(7) Uani 1 1 d . . .
C5 C -0.1092(2) -0.0994(4) 0.30568(19) 0.0147(7) Uani 1 1 d . . .
C6 C -0.1732(2) 0.0110(4) 0.26983(19) 0.0158(7) Uani 1 1 d . . .
N6 N -0.25819(18) -0.0220(4) 0.23689(17) 0.0195(7) Uani 1 1 d . . .
H6A H -0.2959 0.0514 0.2156 0.023 Uiso 1 1 calc R . .
H6B H -0.2768 -0.1174 0.2364 0.023 Uiso 1 1 calc R . .
N7 N -0.11747(19) -0.2563(3) 0.31583(17) 0.0175(6) Uani 1 1 d . . .
C8 C -0.0377(2) -0.3002(4) 0.3554(2) 0.0183(7) Uani 1 1 d . . .
H8 H -0.0232 -0.4035 0.3710 0.022 Uiso 1 1 calc R . .
N9 N 0.02322(18) -0.1828(3) 0.37244(17) 0.0162(6) Uani 1 1 d . . .
C10 C 0.1187(2) -0.2110(4) 0.4075(2) 0.0207(8) Uani 1 1 d . . .
H10A H 0.1506 -0.1554 0.3784 0.025 Uiso 1 1 calc R . .
H10B H 0.1300 -0.3222 0.4039 0.025 Uiso 1 1 calc R . .
C11 C 0.1570(2) -0.1628(4) 0.4887(2) 0.0243(9) Uani 1 1 d . . .
H11A H 0.2222 -0.1738 0.5051 0.029 Uiso 1 1 calc R . .
H11B H 0.1346 -0.2331 0.5196 0.029 Uiso 1 1 calc R . .
S12 S 0.12985(5) 0.03442(10) 0.50583(5) 0.01801(19) Uani 1 1 d . . .
C13 C 0.2320(2) 0.0906(5) 0.5781(2) 0.0254(9) Uani 1 1 d . . .
H13A H 0.2187 0.1718 0.6096 0.030 Uiso 1 1 calc R . .
H13B H 0.2560 0.0008 0.6108 0.030 Uiso 1 1 calc R . .
C14 C 0.3004(3) 0.1482(5) 0.5475(2) 0.0276(9) Uani 1 1 d . . .
H14A H 0.3199 0.0633 0.5217 0.033 Uiso 1 1 calc R . .
H14B H 0.3525 0.1843 0.5892 0.033 Uiso 1 1 calc R . .
S15 S 0.25792(6) 0.30550(12) 0.48178(6) 0.0264(2) Uani 1 1 d . . .
C16 C 0.2451(3) 0.4509(5) 0.5448(3) 0.0396(11) Uani 1 1 d . . .
H16A H 0.2062 0.4127 0.5715 0.059 Uiso 1 1 calc R . .
H16B H 0.2190 0.5432 0.5163 0.059 Uiso 1 1 calc R . .
H16C H 0.3031 0.4763 0.5810 0.059 Uiso 1 1 calc R . .
O17 O 0.4584(2) 0.3787(4) 0.6281(2) 0.0528(10) Uani 1 1 d . . .
C18 C 0.5385(3) 0.3587(5) 0.6558(3) 0.0305(10) Uani 1 1 d . . .
H18 H 0.5622 0.3579 0.7089 0.037 Uiso 1 1 calc R . .
N19 N 0.5949(2) 0.3382(4) 0.6191(2) 0.0322(8) Uani 1 1 d . . .
C20 C 0.5653(5) 0.3265(10) 0.5381(3) 0.085(2) Uani 1 1 d . . .
H20A H 0.5005 0.3207 0.5189 0.127 Uiso 1 1 calc R . .
H20B H 0.5903 0.2337 0.5235 0.127 Uiso 1 1 calc R . .
H20C H 0.5849 0.4172 0.5172 0.127 Uiso 1 1 calc R . .
C21 C 0.6889(3) 0.3207(6) 0.6593(3) 0.0525(14) Uani 1 1 d . . .
H21A H 0.7212 0.4080 0.6480 0.079 Uiso 1 1 calc R . .
H21B H 0.7102 0.2250 0.6437 0.079 Uiso 1 1 calc R . .
H21C H 0.6989 0.3172 0.7133 0.079 Uiso 1 1 calc R . .
O22 O 0.36665(19) 0.8146(4) 0.59981(19) 0.0425(8) Uani 1 1 d . . .
C23 C 0.4351(3) 0.7569(5) 0.6417(2) 0.0296(9) Uani 1 1 d . . .
H23 H 0.4294 0.6662 0.6677 0.036 Uiso 1 1 calc R . .
N24 N 0.5163(2) 0.8102(4) 0.65377(19) 0.0276(8) Uani 1 1 d . . .
C25 C 0.5937(3) 0.7372(5) 0.7062(3) 0.0367(11) Uani 1 1 d . . .
H25A H 0.5752 0.6478 0.7290 0.055 Uiso 1 1 calc R . .
H25B H 0.6243 0.8107 0.7455 0.055 Uiso 1 1 calc R . .
H25C H 0.6338 0.7038 0.6796 0.055 Uiso 1 1 calc R . .
C26 C 0.5317(3) 0.9499(6) 0.6188(3) 0.0463(13) Uani 1 1 d . . .
H26A H 0.5692 0.9276 0.5881 0.069 Uiso 1 1 calc R . .
H26B H 0.5614 1.0251 0.6575 0.069 Uiso 1 1 calc R . .
H26C H 0.4750 0.9920 0.5869 0.069 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
Rh Rh -1.1178 0.9187 '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 Rh1 Cl2 87.56(3) . . ?
Cl1 Rh1 Cl3 176.20(3) . . ?
Cl1 Rh1 N3 95.55(8) . . ?
Cl1 Rh1 S12 99.40(3) . . ?
Cl1 Rh1 S15 81.02(4) . . ?
Cl2 Rh1 Cl3 89.93(3) . . ?
Cl2 Rh1 N3 93.03(8) . . ?
Cl2 Rh1 S12 172.07(3) . . ?
Cl2 Rh1 S15 87.61(3) . . ?
Cl3 Rh1 N3 87.44(8) . . ?
Cl3 Rh1 S12 82.92(3) . . ?
Cl3 Rh1 S15 96.02(4) . . ?
N3 Rh1 S12 90.10(8) . . ?
N3 Rh1 S15 176.49(8) . . ?
S12 Rh1 S15 89.72(3) . . ?
C2 N1 C6 118.8(3) . . ?
N1 C2 N3 128.8(3) . . ?
Rh1 N3 C2 116.6(2) . . ?
Rh1 N3 C4 129.4(2) . . ?
C2 N3 C4 112.4(3) . . ?
N3 C4 C5 123.5(3) . . ?
N3 C4 N9 131.1(3) . . ?
C5 C4 N9 105.5(3) . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 N7 110.4(3) . . ?
C6 C5 N7 130.6(3) . . ?
N1 C6 C5 117.6(3) . . ?
N1 C6 N6 119.0(3) . . ?
C5 C6 N6 123.4(3) . . ?
C5 N7 C8 104.3(3) . . ?
N7 C8 N9 113.6(3) . . ?
C4 N9 C8 106.2(3) . . ?
C4 N9 C10 130.9(3) . . ?
C8 N9 C10 122.2(3) . . ?
N9 C10 C11 115.1(3) . . ?
C10 C11 S12 113.6(2) . . ?
Rh1 S12 C11 113.90(14) . . ?
Rh1 S12 C13 102.30(14) . . ?
C11 S12 C13 100.26(17) . . ?
S12 C13 C14 113.2(3) . . ?
C13 C14 S15 111.2(3) . . ?
Rh1 S15 C14 100.08(13) . . ?
Rh1 S15 C16 112.34(16) . . ?
C14 S15 C16 100.1(2) . . ?
O17 C18 N19 126.5(4) . . ?
C18 N19 C20 121.4(5) . . ?
C18 N19 C21 120.6(4) . . ?
C20 N19 C21 117.9(5) . . ?
O22 C23 N24 125.8(4) . . ?
C23 N24 C25 122.1(4) . . ?
C23 N24 C26 121.3(4) . . ?
C25 N24 C26 116.4(4) . . ?
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
Rh1 Cl1 2.3546(9) . ?
Rh1 Cl2 2.3688(9) . ?
Rh1 Cl3 2.3366(9) . ?
Rh1 N3 2.129(3) . ?
Rh1 S12 2.3064(9) . ?
Rh1 S15 2.3036(10) . ?
N1 C2 1.326(4) . ?
N1 C6 1.357(5) . ?
C2 N3 1.347(4) . ?
N3 C4 1.364(4) . ?
C4 C5 1.392(5) . ?
C4 N9 1.374(4) . ?
C5 C6 1.404(5) . ?
C5 N7 1.390(5) . ?
C6 N6 1.327(4) . ?
N7 C8 1.306(4) . ?
C8 N9 1.375(4) . ?
N9 C10 1.472(4) . ?
C10 C11 1.513(5) . ?
C11 S12 1.824(4) . ?
S12 C13 1.818(4) . ?
C13 C14 1.484(6) . ?
C14 S15 1.822(4) . ?
S15 C16 1.794(5) . ?
O17 C18 1.226(5) . ?
C18 N19 1.319(5) . ?
N19 C20 1.449(7) . ?
N19 C21 1.453(6) . ?
O22 C23 1.227(5) . ?
C23 N24 1.327(5) . ?
N24 C25 1.453(5) . ?
N24 C26 1.443(6) . ?
