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#$Date: 2016-03-23 22:01:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179463 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/60/4336044.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_4336044
loop_
_publ_author_name
'Danila Vasilchenko'
'Sergey Tkachev'
'Iraida Baidina'
'Sergey Korenev'
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       vasilchenko@niic.nsc.ru
_publ_contact_author_fax         7(383)3309489
_publ_contact_author_name        'Vasilchenko Danila Bor.'
_publ_contact_author_phone       7(383)3391633
_publ_section_title
;
 Speciation of Platinum(IV) in Nitric Acid Solutions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10532
_journal_page_last               10541
_journal_paper_doi               10.1021/ic401499j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C4 H12 N, 0.5(H2 N8 O26 Pt2)'
_chemical_formula_sum            'C4 H13 N5 O13 Pt'
_chemical_formula_weight         534.28
_chemical_name_systematic        ?
_chemical_properties_physical    moisture-sensitive
_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                 104.1690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6907(3)
_cell_length_b                   14.8950(5)
_cell_length_c                   13.1091(4)
_cell_measurement_reflns_used    6050
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.96
_cell_measurement_theta_min      2.73
_cell_volume                     1456.00(9)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ 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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12151
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         31.97
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    9.718
_exptl_absorpt_correction_T_max  0.6972
_exptl_absorpt_correction_T_min  0.4750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_recrystallization_method 'nitric acid'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.042
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0222P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                4353
_reflns_number_total             5034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401499j_si_001.cif
_cod_data_source_block           v
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336044
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
Pt1 Pt 0.414772(10) 0.018742(6) 0.881166(6) 0.01011(3) Uani 1 1 d .
O1 O 0.6448(2) -0.02852(11) 0.97674(13) 0.0120(3) Uani 1 1 d D
O31 O 0.4794(2) 0.02684(12) 0.74339(14) 0.0175(3) Uani 1 1 d .
O12 O 0.0255(2) -0.01329(13) 0.87935(16) 0.0215(4) Uani 1 1 d .
O41 O 0.4749(2) 0.14978(11) 0.89372(13) 0.0147(3) Uani 1 1 d .
O21 O 0.3481(2) -0.11108(11) 0.88070(13) 0.0142(3) Uani 1 1 d .
O11 O 0.1859(2) 0.07117(11) 0.79527(13) 0.0150(3) Uani 1 1 d .
O23 O 0.1929(2) -0.10319(13) 0.71385(14) 0.0219(4) Uani 1 1 d .
O33 O 0.6196(2) -0.10407(13) 0.76507(15) 0.0245(4) Uani 1 1 d .
O32 O 0.5608(3) -0.03504(16) 0.61442(15) 0.0288(5) Uani 1 1 d .
O42 O 0.7675(2) 0.12570(12) 0.91434(15) 0.0200(4) Uani 1 1 d .
O43 O 0.6600(3) 0.26050(12) 0.91411(16) 0.0262(4) Uani 1 1 d .
O22 O 0.2292(2) -0.23007(13) 0.79832(15) 0.0249(4) Uani 1 1 d .
N1 N 0.0271(3) 0.03440(14) 0.80330(17) 0.0164(4) Uani 1 1 d .
N3 N 0.5593(3) -0.04319(15) 0.70650(17) 0.0187(4) Uani 1 1 d .
N2 N 0.2501(3) -0.14986(14) 0.79092(16) 0.0156(4) Uani 1 1 d .
N4 N 0.6451(3) 0.17927(14) 0.90802(16) 0.0165(4) Uani 1 1 d .
O13 O -0.0990(2) 0.05525(15) 0.73267(15) 0.0272(4) Uani 1 1 d .
N5 N 0.8147(3) -0.19186(14) 0.46972(16) 0.0161(4) Uani 1 1 d .
C2 C 0.8689(4) -0.09557(18) 0.4772(2) 0.0241(5) Uani 1 1 d .
H2A H 0.9981 -0.0910 0.5084 0.052(12) Uiso 1 1 calc R
H2B H 0.8036 -0.0635 0.5215 0.045(10) Uiso 1 1 calc R
H2C H 0.8405 -0.0689 0.4067 0.033(9) Uiso 1 1 calc R
C3 C 0.8580(4) -0.2331(2) 0.5775(2) 0.0261(6) Uani 1 1 d .
H3A H 0.9872 -0.2287 0.6086 0.034(9) Uiso 1 1 calc R
H3B H 0.8221 -0.2964 0.5722 0.050(11) Uiso 1 1 calc R
H3C H 0.7929 -0.2011 0.6219 0.054(12) Uiso 1 1 calc R
C4 C 0.6177(3) -0.1997(2) 0.4220(2) 0.0274(6) Uani 1 1 d .
H4A H 0.5902 -0.1763 0.3499 0.025(8) Uiso 1 1 calc R
H4B H 0.5519 -0.1651 0.4639 0.039(10) Uiso 1 1 calc R
H4C H 0.5820 -0.2629 0.4208 0.041(10) Uiso 1 1 calc R
C1 C 0.9147(4) -0.2404(2) 0.4023(2) 0.0300(6) Uani 1 1 d .
H1A H 1.0439 -0.2341 0.4325 0.028(8) Uiso 1 1 calc R
H1B H 0.8837 -0.2148 0.3313 0.047(11) Uiso 1 1 calc R
H1C H 0.8821 -0.3041 0.3989 0.035(9) Uiso 1 1 calc R
H1 H 0.737(4) 0.009(2) 0.970(3) 0.024(9) Uiso 1 1 d 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'
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'
Pt Pt -1.7033 8.3905 '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
O31 Pt1 O21 100.17(7) . .
O31 Pt1 O11 81.16(7) . .
O21 Pt1 O11 100.72(7) . .
O31 Pt1 O41 84.92(7) . .
O21 Pt1 O41 174.89(6) . .
O11 Pt1 O41 79.61(7) . .
O31 Pt1 O1 102.00(7) . .
O21 Pt1 O1 81.40(7) . .
O11 Pt1 O1 175.89(7) . .
O41 Pt1 O1 97.96(7) . .
O31 Pt1 O1 172.29(7) . 3_657
O21 Pt1 O1 87.53(6) . 3_657
O11 Pt1 O1 97.08(7) . 3_657
O41 Pt1 O1 87.38(7) . 3_657
O1 Pt1 O1 79.44(7) . 3_657
O31 Pt1 Pt1 141.22(5) . 3_657
O21 Pt1 Pt1 82.81(5) . 3_657
O11 Pt1 Pt1 136.74(5) . 3_657
O41 Pt1 Pt1 93.45(5) . 3_657
O1 Pt1 Pt1 39.74(5) . 3_657
O1 Pt1 Pt1 39.70(4) 3_657 3_657
Pt1 O1 Pt1 100.56(7) . 3_657
Pt1 O1 H1 108(2) . .
Pt1 O1 H1 113(2) 3_657 .
N3 O31 Pt1 120.77(15) . .
N4 O41 Pt1 121.69(13) . .
N2 O21 Pt1 120.01(13) . .
N1 O11 Pt1 118.69(14) . .
O13 N1 O12 127.4(2) . .
O13 N1 O11 113.8(2) . .
O12 N1 O11 118.81(19) . .
O33 N3 O32 127.7(2) . .
O33 N3 O31 119.2(2) . .
O32 N3 O31 113.1(2) . .
O22 N2 O23 127.0(2) . .
O22 N2 O21 113.9(2) . .
O23 N2 O21 119.13(19) . .
O43 N4 O42 126.0(2) . .
O43 N4 O41 113.92(19) . .
O42 N4 O41 120.1(2) . .
C2 N5 C1 109.2(2) . .
C2 N5 C4 110.0(2) . .
C1 N5 C4 109.3(2) . .
C2 N5 C3 109.7(2) . .
C1 N5 C3 109.3(2) . .
C4 N5 C3 109.31(19) . .
N5 C2 H2A 109.5 . .
N5 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N5 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N5 C3 H3A 109.5 . .
N5 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N5 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N5 C4 H4A 109.5 . .
N5 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N5 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N5 C1 H1A 109.5 . .
N5 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N5 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 O31 1.9908(17) .
Pt1 O21 2.0002(16) .
Pt1 O11 2.0013(15) .
Pt1 O41 2.0033(16) .
Pt1 O1 2.0275(16) .
Pt1 O1 2.0295(16) 3_657
Pt1 Pt1 3.12056(18) 3_657
O1 Pt1 2.0295(16) 3_657
O1 H1 0.92(3) .
O31 N3 1.358(3) .
O12 N1 1.227(3) .
O41 N4 1.349(2) .
O21 N2 1.361(2) .
O11 N1 1.366(2) .
O23 N2 1.217(3) .
O33 N3 1.205(3) .
O32 N3 1.216(3) .
O42 N4 1.221(3) .
O43 N4 1.216(3) .
O22 N2 1.212(3) .
N1 O13 1.206(3) .
N5 C2 1.490(3) .
N5 C1 1.493(3) .
N5 C4 1.495(3) .
N5 C3 1.501(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
