#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:49:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179426 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/23/4332312.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332312
loop_
_publ_author_name
'Khripun, Anatoly V.'
'Kukushkin, Vadim Yu.'
'Selivanov, Stanislav I.'
'Haukka, Matti'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Unusual Reaction between (Nitrile)Pt Complexes and Pyrazoles: 
 Substitution Proceeds via Metal-Mediated Nitrile−Pyrazole Coupling
 Followed by Elimination of the Nitrile
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5073
_journal_page_last               5083
_journal_paper_doi               10.1021/ic0602300
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C6 H9 Cl2 N3 Pt, H2 O'
_chemical_formula_sum            'C6 H11 Cl2 N3 O Pt'
_chemical_formula_weight         407.17
_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                 94.288(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3045(6)
_cell_length_b                   10.5777(11)
_cell_length_c                   13.5023(14)
_cell_measurement_reflns_used    7161
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.45
_cell_volume                     1040.33(18)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1a (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7161
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    13.966
_exptl_absorpt_correction_T_max  0.7042
_exptl_absorpt_correction_T_min  0.1575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.14 (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0326
_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)+(0.0183P)²+0.3180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                1620
_reflns_number_total             2113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0602300sup1.cif
_cod_data_source_block           compd_4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4332312
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
Pt1 Pt 0.19876(3) 0.10376(3) 0.47373(2) 0.01782(10) Uani 1 1 d .
Cl1 Cl 0.1602(3) 0.31531(17) 0.50786(15) 0.0291(5) Uani 1 1 d .
Cl2 Cl 0.0768(2) 0.13341(17) 0.31359(14) 0.0256(4) Uani 1 1 d .
O99 O 0.1422(7) -0.1521(5) 0.2562(4) 0.0284(13) Uani 1 1 d .
H99A H 0.1269 -0.0692 0.2352 0.043 Uiso 1 1 d .
H99B H 0.2267 -0.1847 0.2119 0.043 Uiso 1 1 d .
N1 N 0.2417(7) -0.0814(6) 0.4588(5) 0.0209(14) Uani 1 1 d .
H1 H 0.2149 -0.1197 0.4017 0.025 Uiso 1 1 calc R
N2 N 0.3034(7) 0.0594(5) 0.6092(5) 0.0187(14) Uani 1 1 d .
N3 N 0.3460(7) -0.0662(5) 0.6186(5) 0.0187(14) Uani 1 1 d .
C1 C 0.3094(9) -0.1430(6) 0.5345(6) 0.0186(16) Uani 1 1 d .
C2 C 0.3437(10) -0.2793(6) 0.5449(5) 0.0215(17) Uani 1 1 d .
H2A H 0.2555 -0.3154 0.5894 0.026 Uiso 1 1 calc R
H2B H 0.4687 -0.2923 0.5768 0.026 Uiso 1 1 calc R
C3 C 0.3267(10) -0.3510(7) 0.4464(6) 0.0240(18) Uani 1 1 d .
H3A H 0.2068 -0.3332 0.4117 0.036 Uiso 1 1 calc R
H3B H 0.3380 -0.4420 0.4593 0.036 Uiso 1 1 calc R
H3C H 0.4243 -0.3238 0.4052 0.036 Uiso 1 1 calc R
C4 C 0.4162(9) -0.0905(7) 0.7134(5) 0.0203(16) Uani 1 1 d .
H4 H 0.4574 -0.1702 0.7387 0.024 Uiso 1 1 calc R
C5 C 0.4164(10) 0.0205(7) 0.7648(6) 0.0243(17) Uani 1 1 d .
H5 H 0.4558 0.0334 0.8327 0.029 Uiso 1 1 calc R
C6 C 0.3460(9) 0.1119(7) 0.6964(6) 0.0250(18) Uani 1 1 d .
H6 H 0.3314 0.1990 0.7110 0.030 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01479(14) 0.01820(16) 0.02038(17) 0.00215(15) 0.00058(10) 0.00028(14)
Cl1 0.0286(10) 0.0186(9) 0.0393(13) -0.0034(9) -0.0015(8) 0.0037(8)
Cl2 0.0273(10) 0.0277(10) 0.0214(11) 0.0049(8) -0.0022(8) 0.0033(8)
O99 0.033(3) 0.023(3) 0.029(3) -0.006(2) -0.001(2) 0.005(2)
N1 0.016(3) 0.030(4) 0.017(4) -0.003(3) -0.001(3) -0.005(3)
N2 0.014(3) 0.015(3) 0.027(4) -0.001(3) 0.004(3) 0.003(2)
N3 0.017(3) 0.015(3) 0.024(4) 0.001(3) -0.001(3) 0.001(2)
C1 0.018(3) 0.020(4) 0.017(4) -0.004(3) -0.004(3) -0.004(3)
C2 0.027(4) 0.019(4) 0.018(4) 0.001(3) 0.001(3) -0.007(3)
C3 0.028(4) 0.018(4) 0.026(5) -0.004(3) 0.000(3) -0.001(3)
C4 0.021(4) 0.016(4) 0.023(4) 0.001(3) -0.003(3) 0.001(3)
C5 0.023(4) 0.032(4) 0.016(4) -0.005(4) -0.004(3) 0.003(4)
C6 0.020(4) 0.024(4) 0.032(5) -0.006(4) 0.003(3) -0.007(3)
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'
Cl Cl 0.1484 0.1585 '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
N2 Pt1 N1 79.0(2)
N2 Pt1 Cl2 174.18(17)
N1 Pt1 Cl2 95.26(18)
N2 Pt1 Cl1 95.13(17)
N1 Pt1 Cl1 174.10(18)
Cl2 Pt1 Cl1 90.63(7)
H99A O99 H99B 102.6
C1 N1 Pt1 118.2(5)
C1 N1 H1 120.9
Pt1 N1 H1 120.9
C6 N2 N3 106.8(6)
C6 N2 Pt1 140.6(5)
N3 N2 Pt1 112.6(4)
C4 N3 N2 109.6(6)
C4 N3 C1 133.1(6)
N2 N3 C1 117.2(6)
N1 C1 N3 113.0(6)
N1 C1 C2 129.0(7)
N3 C1 C2 118.0(6)
C1 C2 C3 113.7(6)
C1 C2 H2A 108.8
C3 C2 H2A 108.8
C1 C2 H2B 108.8
C3 C2 H2B 108.8
H2A C2 H2B 107.7
C2 C3 H3A 109.5
C2 C3 H3B 109.5
H3A C3 H3B 109.5
C2 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
C5 C4 N3 107.5(6)
C5 C4 H4 126.2
N3 C4 H4 126.2
C4 C5 C6 105.7(7)
C4 C5 H5 127.2
C6 C5 H5 127.2
N2 C6 C5 110.3(7)
N2 C6 H6 124.8
C5 C6 H6 124.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 N2 1.985(6)
Pt1 N1 1.996(6)
Pt1 Cl2 2.2977(19)
Pt1 Cl1 2.3062(19)
O99 H99A 0.9269
O99 H99B 0.9555
N1 C1 1.279(9)
N1 H1 0.8800
N2 C6 1.318(9)
N2 N3 1.369(8)
N3 C4 1.367(9)
N3 C1 1.405(9)
C1 C2 1.469(10)
C2 C3 1.527(10)
C2 H2A 0.9900
C2 H2B 0.9900
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 C5 1.365(10)
C4 H4 0.9500
C5 C6 1.408(10)
C5 H5 0.9500
C6 H6 0.9500
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
O99 H99A Cl2 0.93 2.43 3.163(5) 136.1 .
O99 H99B Cl2 0.96 2.44 3.246(5) 141.9 2_545
