#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/41/2234106.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2234106
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 Bis(di-2-pyridylamine-κ²N²,N^2'^)platinum(II)
 dibromide monohydrate
;
_journal_coeditor_code           BQ2347
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m518
_journal_paper_doi               10.1107/S1600536812013062
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pt (C10 H9 N3)2] Br2, H2 O'
_chemical_formula_moiety         'C20 H18 N6 Pt, 2(Br), H2 O'
_chemical_formula_sum            'C20 H20 Br2 N6 O Pt'
_chemical_formula_weight         715.33
_chemical_name_systematic
;
Bis(di-2-pyridylamine-κ²N²,N^2'^)platinum(II) dibromide
monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.448(2)
_cell_angle_beta                 104.538(2)
_cell_angle_gamma                107.980(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7870(9)
_cell_length_b                   11.0590(10)
_cell_length_c                   12.1151(12)
_cell_measurement_reflns_used    4253
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.17
_cell_volume                     1080.70(18)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6721
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.214
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.745282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0292
_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)+(0.0253P)²+0.3123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3411
_reflns_number_total             4109
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bq2347.cif
_cod_data_source_block           global
_cod_database_code               2234106
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pt Pt1 0.0000 0.5000 0.0000 0.02139(9) Uani d S 1 2
N N1 0.1711(5) 0.4350(5) 0.0277(4) 0.0240(11) Uani d . 1 1
N N2 0.3215(5) 0.6364(5) 0.2257(5) 0.0269(11) Uani d . 1 1
H H2N 0.4183 0.7004 0.2890 0.040 Uiso d R 1 1
N N3 0.0561(5) 0.5768(5) 0.1905(4) 0.0246(11) Uani d . 1 1
C C1 0.1575(7) 0.3112(6) -0.0598(6) 0.0298(14) Uani d . 1 1
H H1 0.0581 0.2463 -0.1264 0.036 Uiso calc R 1 1
C C2 0.2805(7) 0.2766(6) -0.0557(6) 0.0312(15) Uani d . 1 1
H H2 0.2676 0.1907 -0.1194 0.037 Uiso calc R 1 1
C C3 0.4250(8) 0.3699(7) 0.0437(6) 0.0344(15) Uani d . 1 1
H H3 0.5136 0.3506 0.0470 0.041 Uiso calc R 1 1
C C4 0.4381(7) 0.4897(6) 0.1368(6) 0.0291(14) Uani d . 1 1
H H4 0.5354 0.5527 0.2067 0.035 Uiso calc R 1 1
C C5 0.3093(7) 0.5189(6) 0.1287(5) 0.0243(13) Uani d . 1 1
C C6 0.2076(7) 0.6479(6) 0.2715(5) 0.0244(13) Uani d . 1 1
C C7 0.2502(7) 0.7317(6) 0.4000(6) 0.0298(14) Uani d . 1 1
H H7 0.3575 0.7840 0.4560 0.036 Uiso calc R 1 1
C C8 0.1366(8) 0.7384(7) 0.4452(6) 0.0372(16) Uani d . 1 1
H H8 0.1643 0.7999 0.5317 0.045 Uiso calc R 1 1
C C9 -0.0200(7) 0.6543(6) 0.3636(6) 0.0329(15) Uani d . 1 1
H H9 -0.1002 0.6529 0.3946 0.039 Uiso calc R 1 1
C C10 -0.0555(7) 0.5748(6) 0.2397(6) 0.0302(14) Uani d . 1 1
H H10 -0.1621 0.5150 0.1845 0.036 Uiso calc R 1 1
Pt Pt2 1.0000 0.0000 0.0000 0.01798(9) Uani d S 1 2
N N4 1.0831(5) 0.1819(4) 0.1611(4) 0.0220(11) Uani d . 1 1
N N5 0.8237(5) 0.1494(5) 0.1336(4) 0.0235(11) Uani d . 1 1
H H5N 0.7698 0.1868 0.1763 0.035 Uiso d R 1 1
N N6 0.8306(5) 0.0536(4) -0.0701(4) 0.0203(10) Uani d . 1 1
C C11 1.2399(7) 0.2590(6) 0.2295(5) 0.0245(13) Uani d . 1 1
H H11 1.3090 0.2334 0.1944 0.029 Uiso calc R 1 1
C C12 1.3011(7) 0.3710(6) 0.3461(5) 0.0267(14) Uani d . 1 1
H H12 1.4110 0.4235 0.3918 0.032 Uiso calc R 1 1
C C13 1.1976(7) 0.4073(6) 0.3976(6) 0.0295(14) Uani d . 1 1
H H13 1.2371 0.4832 0.4803 0.035 Uiso calc R 1 1
C C14 1.0396(7) 0.3330(5) 0.3281(5) 0.0247(13) Uani d . 1 1
H H14 0.9686 0.3570 0.3617 0.030 Uiso calc R 1 1
C C15 0.9845(6) 0.2211(5) 0.2068(5) 0.0203(12) Uani d . 1 1
C C16 0.7593(6) 0.1050(5) 0.0029(5) 0.0208(12) Uani d . 1 1
C C17 0.6218(7) 0.1153(6) -0.0491(6) 0.0260(13) Uani d . 1 1
H H17 0.5704 0.1472 0.0033 0.031 Uiso calc R 1 1
C C18 0.5612(7) 0.0790(6) -0.1767(6) 0.0288(14) Uani d . 1 1
H H18 0.4653 0.0821 -0.2139 0.035 Uiso calc R 1 1
C C19 0.6406(7) 0.0379(6) -0.2507(6) 0.0272(14) Uani d . 1 1
H H19 0.6047 0.0192 -0.3378 0.033 Uiso calc R 1 1
C C20 0.7725(7) 0.0247(5) -0.1956(5) 0.0243(13) Uani d . 1 1
H H20 0.8258 -0.0057 -0.2469 0.029 Uiso calc R 1 1
Br Br1 0.31515(7) 0.15218(7) 0.57090(7) 0.04448(19) Uani d . 1 1
Br Br2 0.63618(7) 0.30058(6) 0.27528(6) 0.02942(15) Uani d . 1 1
O O1 0.9598(6) 0.0001(6) 0.3324(5) 0.0680(17) Uani d . 1 1
H H1A 0.9056 -0.0343 0.3676 0.102 Uiso d R 1 1
H H1B 1.0433 0.0410 0.3975 0.102 Uiso d R 1 1
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'
Br Br -0.2901 2.4595 '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'
Pt Pt -1.7033 8.3905 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pt1 N1 2_565 . 180.0000(10) ?
N1 Pt1 N3 2_565 2_565 87.10(19) ?
N1 Pt1 N3 . 2_565 92.90(19) ?
N1 Pt1 N3 2_565 . 92.90(19) ?
N1 Pt1 N3 . . 87.10(19) y
N3 Pt1 N3 2_565 . 180.00(11) ?
C5 N1 C1 . . 117.5(5) ?
C5 N1 Pt1 . . 120.7(4) ?
C1 N1 Pt1 . . 121.6(4) ?
C5 N2 C6 . . 127.0(5) ?
C5 N2 H2N . . 119.1 ?
C6 N2 H2N . . 109.0 ?
C6 N3 C10 . . 118.5(5) ?
C6 N3 Pt1 . . 119.5(4) ?
C10 N3 Pt1 . . 121.4(4) ?
C2 C1 N1 . . 122.9(5) ?
C2 C1 H1 . . 118.5 ?
N1 C1 H1 . . 118.5 ?
C1 C2 C3 . . 118.5(6) ?
C1 C2 H2 . . 120.7 ?
C3 C2 H2 . . 120.7 ?
C4 C3 C2 . . 119.3(6) ?
C4 C3 H3 . . 120.4 ?
C2 C3 H3 . . 120.4 ?
C3 C4 C5 . . 119.8(6) ?
C3 C4 H4 . . 120.1 ?
C5 C4 H4 . . 120.1 ?
N1 C5 N2 . . 118.9(5) ?
N1 C5 C4 . . 121.6(5) ?
N2 C5 C4 . . 119.5(5) ?
N3 C6 N2 . . 119.4(5) ?
N3 C6 C7 . . 120.7(6) ?
N2 C6 C7 . . 119.9(5) ?
C8 C7 C6 . . 119.5(6) ?
C8 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
C7 C8 C9 . . 119.5(6) ?
C7 C8 H8 . . 120.2 ?
C9 C8 H8 . . 120.2 ?
C10 C9 C8 . . 118.7(6) ?
C10 C9 H9 . . 120.7 ?
C8 C9 H9 . . 120.7 ?
C9 C10 N3 . . 122.5(6) ?
C9 C10 H10 . . 118.7 ?
N3 C10 H10 . . 118.7 ?
N6 Pt2 N6 . 2_755 180.0(2) ?
N6 Pt2 N4 . 2_755 93.35(17) ?
N6 Pt2 N4 2_755 2_755 86.65(17) ?
N6 Pt2 N4 . . 86.65(17) y
N6 Pt2 N4 2_755 . 93.35(17) ?
N4 Pt2 N4 2_755 . 180.0(3) ?
C15 N4 C11 . . 119.4(5) ?
C15 N4 Pt2 . . 120.3(4) ?
C11 N4 Pt2 . . 120.2(4) ?
C16 N5 C15 . . 123.2(5) ?
C16 N5 H5N . . 113.7 ?
C15 N5 H5N . . 111.0 ?
C16 N6 C20 . . 117.8(5) ?
C16 N6 Pt2 . . 120.3(4) ?
C20 N6 Pt2 . . 121.6(4) ?
C12 C11 N4 . . 122.4(5) ?
C12 C11 H11 . . 118.8 ?
N4 C11 H11 . . 118.8 ?
C11 C12 C13 . . 118.3(5) ?
C11 C12 H12 . . 120.9 ?
C13 C12 H12 . . 120.9 ?
C14 C13 C12 . . 119.8(5) ?
C14 C13 H13 . . 120.1 ?
C12 C13 H13 . . 120.1 ?
C13 C14 C15 . . 118.9(5) ?
C13 C14 H14 . . 120.5 ?
C15 C14 H14 . . 120.5 ?
N4 C15 N5 . . 120.0(5) ?
N4 C15 C14 . . 121.0(5) ?
N5 C15 C14 . . 118.9(5) ?
N6 C16 N5 . . 119.7(5) ?
N6 C16 C17 . . 121.6(5) ?
N5 C16 C17 . . 118.7(5) ?
C18 C17 C16 . . 119.5(6) ?
C18 C17 H17 . . 120.3 ?
C16 C17 H17 . . 120.3 ?
C17 C18 C19 . . 119.5(5) ?
C17 C18 H18 . . 120.2 ?
C19 C18 H18 . . 120.2 ?
C20 C19 C18 . . 118.5(6) ?
C20 C19 H19 . . 120.8 ?
C18 C19 H19 . . 120.8 ?
N6 C20 C19 . . 122.8(6) ?
N6 C20 H20 . . 118.6 ?
C19 C20 H20 . . 118.6 ?
H1A O1 H1B . . 93.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 N1 2_565 2.013(5) ?
Pt1 N1 . 2.013(5) y
Pt1 N3 2_565 2.030(5) ?
Pt1 N3 . 2.030(5) y
N1 C5 . 1.351(7) ?
N1 C1 . 1.366(7) ?
N2 C5 . 1.379(7) ?
N2 C6 . 1.384(7) ?
N2 H2N . 0.9200 ?
N3 C6 . 1.348(7) ?
N3 C10 . 1.367(8) ?
C1 C2 . 1.366(8) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.389(8) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.368(8) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.384(8) ?
C4 H4 . 0.9500 ?
C6 C7 . 1.390(8) ?
C7 C8 . 1.369(9) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.392(9) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.348(8) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
Pt2 N6 . 2.014(4) y
Pt2 N6 2_755 2.014(4) ?
Pt2 N4 2_755 2.024(4) ?
Pt2 N4 . 2.024(4) y
N4 C15 . 1.339(7) ?
N4 C11 . 1.361(7) ?
N5 C16 . 1.391(7) ?
N5 C15 . 1.397(7) ?
N5 H5N . 0.9200 ?
N6 C16 . 1.346(7) ?
N6 C20 . 1.367(7) ?
C11 C12 . 1.356(7) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.406(8) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.370(8) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.401(7) ?
C14 H14 . 0.9500 ?
C16 C17 . 1.392(7) ?
C17 C18 . 1.372(8) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.383(8) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.371(8) ?
C19 H19 . 0.9500 ?
C20 H20 . 0.9500 ?
O1 H1A . 0.8400 ?
O1 H1B . 0.8400 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1A Br1 2_656 0.84 2.58 3.399(6) 166.4
O1 H1B Br1 1_655 0.84 2.54 3.374(5) 171.1
N2 H2N Br1 2_666 0.92 2.38 3.289(4) 170.6
N5 H5N Br2 . 0.92 2.35 3.267(4) 173.5
C2 H2 O1 2_655 0.95 2.58 3.302(8) 133.0
C11 H11 Br2 1_655 0.95 2.87 3.635(6) 138.4
C13 H13 Br2 2_766 0.95 2.76 3.712(6) 177.1
C20 H20 O1 2_755 0.95 2.56 3.464(8) 160.1
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
N3 Pt1 N1 C5 2_565 138.4(5)
N3 Pt1 N1 C5 . -41.6(5)
N3 Pt1 N1 C1 2_565 -35.8(5)
N3 Pt1 N1 C1 . 144.2(5)
N1 Pt1 N3 C6 2_565 -136.6(4)
N1 Pt1 N3 C6 . 43.4(4)
N1 Pt1 N3 C10 2_565 34.7(5)
N1 Pt1 N3 C10 . -145.3(5)
C5 N1 C1 C2 . -6.6(9)
Pt1 N1 C1 C2 . 167.8(5)
N1 C1 C2 C3 . 1.7(10)
C1 C2 C3 C4 . 2.7(9)
C2 C3 C4 C5 . -2.1(9)
C1 N1 C5 N2 . -172.9(5)
Pt1 N1 C5 N2 . 12.7(7)
C1 N1 C5 C4 . 7.2(8)
Pt1 N1 C5 C4 . -167.2(5)
C6 N2 C5 N1 . 36.1(8)
C6 N2 C5 C4 . -144.0(6)
C3 C4 C5 N1 . -3.0(9)
C3 C4 C5 N2 . 177.1(6)
C10 N3 C6 N2 . 171.8(5)
Pt1 N3 C6 N2 . -16.6(7)
C10 N3 C6 C7 . -8.0(8)
Pt1 N3 C6 C7 . 163.6(4)
C5 N2 C6 N3 . -33.6(8)
C5 N2 C6 C7 . 146.2(6)
N3 C6 C7 C8 . 2.1(9)
N2 C6 C7 C8 . -177.7(5)
C6 C7 C8 C9 . 4.0(9)
C7 C8 C9 C10 . -4.1(9)
C8 C9 C10 N3 . -2.0(10)
C6 N3 C10 C9 . 8.0(9)
Pt1 N3 C10 C9 . -163.3(5)
N6 Pt2 N4 C15 . 41.4(4)
N6 Pt2 N4 C15 2_755 -138.6(4)
N6 Pt2 N4 C11 . -144.2(4)
N6 Pt2 N4 C11 2_755 35.8(4)
N4 Pt2 N6 C16 2_755 136.8(4)
N4 Pt2 N6 C16 . -43.2(4)
N4 Pt2 N6 C20 2_755 -35.8(4)
N4 Pt2 N6 C20 . 144.2(4)
C15 N4 C11 C12 . 3.2(8)
Pt2 N4 C11 C12 . -171.2(4)
N4 C11 C12 C13 . 0.4(9)
C11 C12 C13 C14 . -2.2(9)
C12 C13 C14 C15 . 0.4(9)
C11 N4 C15 N5 . 175.4(5)
Pt2 N4 C15 N5 . -10.2(7)
C11 N4 C15 C14 . -5.1(8)
Pt2 N4 C15 C14 . 169.4(4)
C16 N5 C15 N4 . -40.2(7)
C16 N5 C15 C14 . 140.2(5)
C13 C14 C15 N4 . 3.3(8)
C13 C14 C15 N5 . -177.2(5)
C20 N6 C16 N5 . -173.5(5)
Pt2 N6 C16 N5 . 13.6(7)
C20 N6 C16 C17 . 6.4(8)
Pt2 N6 C16 C17 . -166.5(4)
C15 N5 C16 N6 . 38.2(7)
C15 N5 C16 C17 . -141.6(5)
N6 C16 C17 C18 . -3.3(9)
N5 C16 C17 C18 . 176.6(5)
C16 C17 C18 C19 . -2.4(9)
C17 C18 C19 C20 . 4.7(9)
C16 N6 C20 C19 . -4.0(8)
Pt2 N6 C20 C19 . 168.8(4)
C18 C19 C20 N6 . -1.5(9)
