#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318380.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_4318380
loop_
_publ_author_name
'Pablo Vitoria'
'Javier I. Beitia'
'Juan Manuel Gutiérrez-Zorrilla'
'Emilio R. Sáiz'
'Antonio Luque'
'Maite Insausti'
'José J. Blanco'
_publ_contact_author
;
  'Juan Manuel Gutierrez-Zorrilla.
  Departamento de Quimica Inorganica. Facultad de Ciencias
  Universidad del Pais Vasco,  Apdo. 644, E-48080 Bilbao, Spain
;
_publ_contact_author_email       qipguloj@lg.ehu.es
_publ_contact_author_fax         '+34-944 648 500'
_publ_contact_author_phone       '+34-946 015 522'
_publ_section_title
;
 Tetracyanometalates of Ni, Pd, and Pt with Cyclic Diquaternary Cations of
 2,2'-Bipyridine and 1,10-Phenanthroline. A Vibrational, Crystallographic,
 and Theoretical Study of Intermolecular Weak Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4396
_journal_page_last               4404
_journal_paper_doi               10.1021/ic0200287
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'aqueous synthesis'
_chemical_formula_moiety         'C14 H12 N2, C4 N4 Pt, H2 O'
_chemical_formula_sum            'C18 H14 N6 O Pt'
_chemical_formula_weight         525.44
_chemical_name_systematic
;
5,6-dihydrodipyrazino[1,2,3,4-lmn]-1,10-phenanthrolinium
  tetracyanoplatinate(ii) hydrate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.928(2)
_cell_length_b                   14.754(2)
_cell_length_c                   12.046(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.65
_cell_measurement_theta_min      5.44
_cell_volume                     1732.2(7)
_computing_cell_refinement       'local programs'
_computing_data_collection       'CAD4 programs'
_computing_data_reduction        'XCAD (Harms and Wocadlo,1995)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4 diffractometer'
_diffrn_measurement_method       'ω/2θ mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5219
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.121
_exptl_absorpt_correction_T_max  0.2894
_exptl_absorpt_correction_T_min  0.0651
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (Walker and Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_meas      2.02(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.087
_refine_diff_density_min         -2.421
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.755
_refine_ls_goodness_of_fit_ref   1.443
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.443
_refine_ls_restrained_S_obs      1.755
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0636P)²+0.0120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0968
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                2441
_reflns_number_total             5029
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0200287_4.cif
_cod_data_source_block           comp6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C18 H14 N6 O1 Pt1'
_cod_database_code               4318380
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pt1 Pt 0 0.5 0.5 0.02978(8) Uani 1 d S .
Pt2 Pt 0.5 0 0.5 0.03219(8) Uani 1 d S .
O1 O 0.3742(3) 0.3062(2) 0.4038(3) 0.0810(10) Uani 1 d . .
N1 N 0.0682(4) 0.3091(2) 0.4142(3) 0.0582(10) Uani 1 d . .
N2 N 0.2494(4) 0.5839(2) 0.4116(3) 0.0608(10) Uani 1 d . .
C1 C 0.0442(4) 0.3776(3) 0.4470(3) 0.0385(8) Uani 1 d . .
C2 C 0.1597(4) 0.5519(2) 0.4430(3) 0.0395(9) Uani 1 d . .
N3 N 0.3808(3) 0.1723(2) 0.5975(3) 0.0562(9) Uani 1 d . .
N4 N 0.7216(4) 0.1238(2) 0.4218(3) 0.0566(9) Uani 1 d . .
C3 C 0.4215(4) 0.1088(3) 0.5621(3) 0.0398(9) Uani 1 d . .
C4 C 0.6399(4) 0.0781(3) 0.4491(3) 0.0396(9) Uani 1 d . .
N11 N 0.8479(3) 0.3352(2) 0.1867(2) 0.0320(7) Uani 1 d . .
C12 C 0.9437(4) 0.2926(2) 0.1454(3) 0.0391(8) Uani 1 d . .
C13 C 1.0527(4) 0.3391(3) 0.1181(3) 0.0483(10) Uani 1 d . .
C14 C 1.0606(3) 0.4301(3) 0.1274(3) 0.0430(9) Uani 1 d . .
C15 C 0.9571(5) 0.4772(3) 0.1669(4) 0.0368(10) Uani 1 d . .
C16 C 0.8533(4) 0.4274(2) 0.2020(3) 0.0275(7) Uani 1 d . .
C17 C 0.9530(4) 0.5740(3) 0.1710(3) 0.0412(10) Uani 1 d . .
C18 C 0.7259(3) 0.2862(2) 0.2089(3) 0.0379(8) Uani 1 d . .
N21 N 0.6567(3) 0.4255(2) 0.2957(3) 0.0327(7) Uani 1 d . .
C22 C 0.5593(4) 0.4663(4) 0.3382(4) 0.0460(10) Uani 1 d . .
C23 C 0.5471(5) 0.5601(3) 0.3359(4) 0.0500(12) Uani 1 d . .
C24 C 0.6405(5) 0.6097(3) 0.2928(4) 0.0460(11) Uani 1 d . .
C25 C 0.7454(3) 0.5689(3) 0.2493(2) 0.0322(9) Uani 1 d . .
C26 C 0.7498(3) 0.4734(4) 0.2494(2) 0.0298(9) Uani 1 d . .
C27 C 0.8476(5) 0.6168(3) 0.2062(3) 0.0427(10) Uani 1 d . .
C28 C 0.6783(4) 0.3248(3) 0.3094(3) 0.0386(9) Uani 1 d . .
H12 H 0.915 0.2262 0.1279 0.05 Uiso 1 d . .
H13 H 1.1154 0.3124 0.0898 0.05 Uiso 1 d . .
H14 H 1.1368 0.4638 0.1013 0.05 Uiso 1 d . .
H17 H 1.0096 0.6083 0.135 0.05 Uiso 1 d . .
H181 H 0.7587 0.2195 0.2309 0.05 Uiso 1 d . .
H182 H 0.6564 0.2858 0.142 0.05 Uiso 1 d . .
H22 H 0.489 0.4279 0.3715 0.05 Uiso 1 d . .
H23 H 0.4895 0.5978 0.3742 0.05 Uiso 1 d . .
H24 H 0.6509 0.6836 0.3032 0.05 Uiso 1 d . .
H27 H 0.8422 0.6874 0.1998 0.05 Uiso 1 d . .
H282 H 0.761 0.3121 0.3902 0.05 Uiso 1 d . .
H281 H 0.5847 0.2984 0.3172 0.05 Uiso 1 d . .
H1 H 0.378 0.2735 0.4698 0.05 Uiso 1 d . .
H2 H 0.2842 0.3131 0.381 0.05 Uiso 1 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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
C1 Pt1 C1 180 3_566 . ?
C1 Pt1 C2 90.0(2) 3_566 . ?
C1 Pt1 C2 89.97(15) . . ?
C1 Pt1 C2 90.0(2) 3_566 3_566 ?
C1 Pt1 C2 90.0(2) . 3_566 ?
C2 Pt1 C2 180 . 3_566 ?
C4 Pt2 C4 180 3_656 . ?
C4 Pt2 C3 89.74(14) 3_656 3_656 ?
C4 Pt2 C3 90.26(14) . 3_656 ?
C4 Pt2 C3 90.26(14) 3_656 . ?
C4 Pt2 C3 89.74(14) . . ?
C3 Pt2 C3 180 3_656 . ?
N1 C1 Pt1 178.2(3) . . ?
N2 C2 Pt1 177.9(4) . . ?
N3 C3 Pt2 177.7(3) . . ?
N4 C4 Pt2 178.6(3) . . ?
C12 N11 C16 120.8(3) . . ?
C12 N11 C18 120.7(3) . . ?
C16 N11 C18 118.2(3) . . ?
N11 C12 C13 120.8(3) . . ?
C14 C13 C12 120.9(4) . . ?
C13 C14 C15 119.2(4) . . ?
C16 C15 C14 118.4(4) . . ?
C16 C15 C17 119.2(4) . . ?
C14 C15 C17 122.4(4) . . ?
N11 C16 C15 119.6(4) . . ?
N11 C16 C26 120.6(4) . . ?
C15 C16 C26 119.8(4) . . ?
C27 C17 C15 120.2(4) . . ?
N11 C18 C28 110.9(3) . . ?
C22 N21 C26 121.7(4) . . ?
C22 N21 C28 120.4(4) . . ?
C26 N21 C28 117.5(4) . . ?
N21 C22 C23 120.9(4) . . ?
C24 C23 C22 118.7(4) . . ?
C23 C24 C25 121.8(4) . . ?
C24 C25 C26 117.2(3) . . ?
C24 C25 C27 124.3(4) . . ?
C26 C25 C27 118.4(3) . . ?
N21 C26 C25 119.6(3) . . ?
N21 C26 C16 120.7(5) . . ?
C25 C26 C16 119.7(3) . . ?
C17 C27 C25 122.2(4) . . ?
C18 C28 N21 110.4(3) . . ?
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
Pt1 C1 1.992(4) 3_566 ?
Pt1 C1 1.992(4) . ?
Pt1 C2 1.996(4) . ?
Pt1 C2 1.996(4) 3_566 ?
Pt2 C4 1.989(4) 3_656 ?
Pt2 C4 1.989(4) . ?
Pt2 C3 1.992(4) 3_656 ?
Pt2 C3 1.992(4) . ?
N1 C1 1.127(4) . ?
N2 C2 1.135(5) . ?
N3 C3 1.135(4) . ?
N4 C4 1.149(5) . ?
N11 C12 1.314(4) . ?
N11 C16 1.372(4) . ?
N11 C18 1.479(4) . ?
C12 C13 1.373(5) . ?
C13 C14 1.348(5) . ?
C14 C15 1.397(6) . ?
C15 C16 1.395(6) . ?
C15 C17 1.431(5) . ?
C16 C26 1.437(5) . ?
C17 C27 1.357(6) . ?
C18 C28 1.495(5) . ?
N21 C22 1.322(5) . ?
N21 C26 1.363(5) . ?
N21 C28 1.506(4) . ?
C22 C23 1.389(7) . ?
C23 C24 1.359(7) . ?
C24 C25 1.389(5) . ?
C25 C26 1.410(6) . ?
C25 C27 1.414(5) . ?
