#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:40:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179072 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/34/4303484.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_4303484
loop_
_publ_author_name
'Miguel A. Galindo'
'David Amantia'
'Alberto Martinez Martinez'
'William Clegg'
'Ross W. Harrington'
'Virtudes Moreno Martinez'
'Andrew Houlton'
_publ_section_title
;
Probing Metal-Ion Purine Interactions at DNA Minor-Groove Sites
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10295
_journal_page_last               10303
_journal_paper_doi               10.1021/ic9013448
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C20 H38 Cd2 Cl2 N18 O7'
_chemical_formula_sum            'C20 H38 Cd2 Cl2 N18 O7'
_chemical_formula_weight         938.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.001(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.5113(8)
_cell_length_b                   7.8916(2)
_cell_length_c                   14.9198(4)
_cell_measurement_reflns_used    71698
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3275.86(16)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25740
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.356
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3759
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0499P)²+32.6375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                3303
_reflns_number_total             3759
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic9013448_si_001_3.cif
_cod_data_source_block           ah101_compound_2
_cod_original_cell_volume        3275.86(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4303484
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Cd1 Cd 0.2500 0.7500 0.5000 0.02120(17) Uani 1 2 d S . .
Cd2 Cd 0.5000 0.62877(6) 0.2500 0.02066(17) Uani 1 2 d S . .
Cl Cl 0.57978(4) 0.49954(17) 0.30464(9) 0.0288(3) Uani 1 1 d . . .
O1 O 0.21246(12) 0.4956(5) 0.4101(3) 0.0297(8) Uani 1 1 d . . .
O2 O 0.21699(17) 0.2544(5) 0.3475(4) 0.0401(10) Uani 1 1 d . . .
O3 O 0.28203(13) 0.3927(5) 0.4447(3) 0.0354(9) Uani 1 1 d . . .
O4 O 0.5000 0.9174(7) 0.2500 0.0270(11) Uani 1 2 d SD . .
H4A H 0.5074(18) 0.967(6) 0.208(3) 0.015(12) Uiso 1 1 d D . .
N1 N 0.61323(13) 0.8481(5) 0.6460(3) 0.0223(8) Uani 1 1 d . . .
N2 N 0.60846(15) 1.0045(6) 0.7704(3) 0.0290(9) Uani 1 1 d D . .
H2A H 0.5932(17) 1.047(9) 0.801(4) 0.05(2) Uiso 1 1 d D . .
H2B H 0.6393(8) 1.027(8) 0.800(4) 0.038(17) Uiso 1 1 d D . .
N3 N 0.53749(13) 0.8967(5) 0.6460(3) 0.0198(8) Uani 1 1 d . . .
N6 N 0.61974(15) 0.7106(6) 0.5167(4) 0.0279(9) Uani 1 1 d D . .
H6A H 0.6507(8) 0.716(7) 0.553(3) 0.027(15) Uiso 1 1 d D . .
H6B H 0.6097(16) 0.647(7) 0.462(3) 0.029(16) Uiso 1 1 d D . .
N7 N 0.50809(13) 0.6693(5) 0.4172(3) 0.0195(8) Uani 1 1 d . . .
N9 N 0.47059(14) 0.7699(5) 0.5018(3) 0.0197(8) Uani 1 1 d . . .
N13 N 0.29727(13) 0.7780(5) 0.4206(3) 0.0201(8) Uani 1 1 d D . .
H13 H 0.295(2) 0.682(5) 0.387(5) 0.045(19) Uiso 1 1 d D . .
N16 N 0.19804(14) 0.8843(5) 0.3484(3) 0.0214(8) Uani 1 1 d D . .
H16A H 0.1680(9) 0.846(5) 0.314(3) 0.000(10) Uiso 1 1 d D . .
H16B H 0.1976(17) 0.989(4) 0.368(5) 0.041(18) Uiso 1 1 d D . .
N17 N 0.23765(15) 0.3782(5) 0.4012(3) 0.0239(8) Uani 1 1 d . . .
C2 C 0.58527(16) 0.9121(6) 0.6846(3) 0.0213(9) Uani 1 1 d . . .
C4 C 0.51827(15) 0.8088(6) 0.5592(3) 0.0178(8) Uani 1 1 d . . .
C5 C 0.54148(17) 0.7458(5) 0.5079(3) 0.0185(9) Uani 1 1 d . . .
C6 C 0.59182(17) 0.7662(6) 0.5567(4) 0.0215(9) Uani 1 1 d . . .
C8 C 0.46677(16) 0.6871(6) 0.4186(4) 0.0211(9) Uani 1 1 d . . .
H8 H 0.4371 0.6457 0.3664 0.025 Uiso 1 1 calc R . .
C10 C 0.43344(16) 0.8103(6) 0.5307(3) 0.0205(9) Uani 1 1 d . . .
H10A H 0.4344 0.9334 0.5442 0.025 Uiso 1 1 calc R . .
H10B H 0.4407 0.7499 0.5945 0.025 Uiso 1 1 calc R . .
C11 C 0.38298(16) 0.7625(6) 0.4502(4) 0.0203(9) Uani 1 1 d . . .
H11A H 0.3813 0.6398 0.4350 0.024 Uiso 1 1 calc R . .
H11B H 0.3743 0.8262 0.3868 0.024 Uiso 1 1 calc R . .
C12 C 0.34849(16) 0.8069(7) 0.4926(4) 0.0238(10) Uani 1 1 d . . .
H12A H 0.3571 0.7383 0.5543 0.029 Uiso 1 1 calc R . .
H12B H 0.3530 0.9276 0.5130 0.029 Uiso 1 1 calc R . .
C14 C 0.27526(17) 0.9158(7) 0.3455(4) 0.0238(10) Uani 1 1 d . . .
H14A H 0.2903 0.9202 0.3003 0.029 Uiso 1 1 calc R . .
H14B H 0.2808 1.0259 0.3810 0.029 Uiso 1 1 calc R . .
C15 C 0.22160(17) 0.8845(7) 0.2829(4) 0.0258(10) Uani 1 1 d . . .
H15A H 0.2072 0.9740 0.2307 0.031 Uiso 1 1 calc R . .
H15B H 0.2162 0.7740 0.2477 0.031 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'
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
O1 Cd1 O1 180.0 . 7_566 ?
O1 Cd1 N13 93.49(14) . . ?
O1 Cd1 N13 86.51(14) . 7_566 ?
O1 Cd1 N13 86.51(14) 7_566 . ?
O1 Cd1 N13 93.49(14) 7_566 7_566 ?
O1 Cd1 N16 84.29(14) . . ?
O1 Cd1 N16 95.71(14) . 7_566 ?
O1 Cd1 N16 84.29(14) 7_566 7_566 ?
O1 Cd1 N16 95.71(14) 7_566 . ?
N13 Cd1 N13 180.0 . 7_566 ?
N13 Cd1 N16 77.71(14) . . ?
N13 Cd1 N16 102.29(14) . 7_566 ?
N13 Cd1 N16 77.71(14) 7_566 7_566 ?
N13 Cd1 N16 102.29(14) 7_566 . ?
N16 Cd1 N16 180.0 . 7_566 ?
Cl Cd2 Cl 131.22(7) . 2_655 ?
Cl Cd2 O4 114.39(3) . . ?
Cl Cd2 O4 114.39(3) 2_655 . ?
Cl Cd2 N7 96.70(10) . . ?
Cl Cd2 N7 89.61(9) 2_655 . ?
Cl Cd2 N7 96.70(10) 2_655 2_655 ?
Cl Cd2 N7 89.61(9) . 2_655 ?
O4 Cd2 N7 82.36(10) . . ?
O4 Cd2 N7 82.36(10) . 2_655 ?
N7 Cd2 N7 164.7(2) . 2_655 ?
Cd1 O1 N17 120.2(3) . . ?
C2 N1 C6 118.5(4) . . ?
C2 N3 C4 111.7(4) . . ?
Cd2 N7 C5 136.4(3) . . ?
Cd2 N7 C8 114.0(3) . . ?
C5 N7 C8 103.7(4) . . ?
C4 N9 C8 106.3(4) . . ?
C4 N9 C10 124.2(4) . . ?
C8 N9 C10 129.5(4) . . ?
Cd1 N13 C12 112.9(3) . . ?
Cd1 N13 C14 105.8(3) . . ?
C12 N13 C14 113.6(4) . . ?
Cd1 N16 C15 107.4(3) . . ?
O1 N17 O2 118.7(4) . . ?
O1 N17 O3 119.1(4) . . ?
O2 N17 O3 122.2(4) . . ?
N1 C2 N2 115.7(4) . . ?
N1 C2 N3 127.3(4) . . ?
N2 C2 N3 117.0(4) . . ?
N3 C4 N9 125.9(4) . . ?
N3 C4 C5 127.5(4) . . ?
N9 C4 C5 106.5(4) . . ?
N7 C5 C4 109.8(4) . . ?
N7 C5 C6 134.5(4) . . ?
C4 C5 C6 115.7(4) . . ?
N1 C6 N6 117.9(4) . . ?
N1 C6 C5 119.1(4) . . ?
N6 C6 C5 123.0(4) . . ?
N7 C8 N9 113.7(4) . . ?
N9 C10 C11 113.4(4) . . ?
C10 C11 C12 107.3(4) . . ?
N13 C12 C11 114.1(4) . . ?
N13 C14 C15 109.7(4) . . ?
N16 C15 C14 110.7(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
Cd1 O1 2.396(4) . ?
Cd1 O1 2.396(4) 7_566 ?
Cd1 N13 2.309(4) . ?
Cd1 N13 2.309(4) 7_566 ?
Cd1 N16 2.333(4) . ?
Cd1 N16 2.333(4) 7_566 ?
Cd2 Cl 2.4698(11) . ?
Cd2 Cl 2.4698(11) 2_655 ?
Cd2 O4 2.278(5) . ?
Cd2 N7 2.406(4) . ?
Cd2 N7 2.406(4) 2_655 ?
O1 N17 1.267(5) . ?
O2 N17 1.238(6) . ?
O3 N17 1.240(6) . ?
N1 C2 1.355(6) . ?
N1 C6 1.344(6) . ?
N2 C2 1.352(6) . ?
N3 C2 1.342(6) . ?
N3 C4 1.337(6) . ?
N6 C6 1.347(6) . ?
N7 C5 1.402(6) . ?
N7 C8 1.320(6) . ?
N9 C4 1.370(6) . ?
N9 C8 1.356(6) . ?
N9 C10 1.461(6) . ?
N13 C12 1.477(6) . ?
N13 C14 1.480(6) . ?
N16 C15 1.479(6) . ?
C4 C5 1.377(6) . ?
C5 C6 1.410(7) . ?
C10 C11 1.523(6) . ?
C11 C12 1.533(6) . ?
C14 C15 1.520(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4A N3 0.858(19) 1.93(2) 2.770(5) 165(5) 6_575
N2 H2B O1 0.876(19) 2.12(3) 2.945(5) 156(6) 8_566
N6 H6A O3 0.867(19) 2.27(4) 2.984(5) 140(4) 5_666
N6 H6B Cl 0.875(19) 2.39(2) 3.260(5) 174(6) .
N13 H13 O3 0.89(2) 2.53(6) 3.126(6) 125(6) .
N16 H16A Cl 0.893(18) 2.97(3) 3.586(4) 127(3) 3_455
N16 H16B O2 0.884(19) 2.24(4) 2.983(6) 142(6) 1_565
