#------------------------------------------------------------------------------
#$Date: 2017-01-11 05:11:36 +0200 (Wed, 11 Jan 2017) $
#$Revision: 190361 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/94/7119405.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_7119405
loop_
_publ_author_name
'Kuwamura, Naoto'
'Kurioka, Yoshinari'
'Konno, Takumi'
_publ_section_title
;
 A platinum(ii)-palladium(ii)-nickel(ii) heterotrimetallic coordination
 polymer showing a cooperative effect on catalytic hydrogen evolution.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              846
_journal_page_last               849
_journal_paper_doi               10.1039/c6cc08789b
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C20 H48 Cl2 N8 Ni O12 Pd2 Pt2 S4, 14(O)'
_chemical_formula_sum            'C20 H48 Cl2 N8 Ni O26 Pd2 Pt2 S4'
_chemical_formula_weight         1677.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-02 deposited with the CCDC.
2016-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.332(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.503(3)
_cell_length_b                   9.0650(10)
_cell_length_c                   18.450(2)
_cell_measurement_reflns_used    10811
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.00
_cell_volume                     3281.1(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12826
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.003
_exptl_absorpt_coefficient_mu    5.342
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, ????)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.900
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.258
_refine_ls_abs_structure_details
;
 Flack x determined using 2217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         7192
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0913P)²+28.2286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1658
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                6107
_reflns_number_total             7192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc08789b2.cif
_cod_data_source_block           PtPdNi_Konno
_cod_original_cell_volume        3281.0(7)
_cod_database_code               7119405
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.617
_shelx_estimated_absorpt_t_max   0.856
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.57460(3) 0.43968(6) 0.50190(3) 0.02405(18) Uani 1 1 d . . . . .
Pd0 Pd 0.41579(5) 0.4323(2) 0.28400(6) 0.0224(3) Uani 1 1 d . . . . .
S11 S 0.6062(2) 0.5604(4) 0.6260(3) 0.0262(9) Uani 1 1 d . . . . .
S9 S 0.5118(2) 0.3144(4) 0.3777(3) 0.0252(8) Uani 1 1 d . . . . .
N3 N 0.6006(7) 0.2351(15) 0.5574(10) 0.029(3) Uani 1 1 d . . . . .
H3A H 0.6409 0.2058 0.5617 0.044 Uiso 1 1 calc R U . . .
H3B H 0.5675 0.1688 0.5261 0.044 Uiso 1 1 calc R U . . .
H3C H 0.6049 0.2402 0.6091 0.044 Uiso 1 1 calc R U . . .
C1 C 0.4938(10) 0.2222(18) 0.2327(11) 0.031(4) Uani 1 1 d . . . . .
H1 H 0.4795 0.1283 0.2481 0.037 Uiso 1 1 calc R U . . .
N0 N 0.4354(8) 0.323(2) 0.1979(9) 0.038(4) Uani 1 1 d . . . . .
H0A H 0.3975 0.2715 0.1628 0.046 Uiso 1 1 calc R U . . .
H0B H 0.4423 0.3927 0.1671 0.046 Uiso 1 1 calc R U . . .
C0 C 0.5532(8) 0.2893(17) 0.3126(11) 0.028(4) Uani 1 1 d . . . . .
O0 O 0.4924(7) 0.2711(14) 0.1067(7) 0.034(3) Uani 1 1 d . . . . .
N2 N 0.5565(8) 0.6402(15) 0.4429(10) 0.035(4) Uani 1 1 d . . . . .
H2A H 0.5965 0.6899 0.4617 0.053 Uiso 1 1 calc R U . . .
H2B H 0.5275 0.6938 0.4536 0.053 Uiso 1 1 calc R U . . .
H2C H 0.5375 0.6257 0.3871 0.053 Uiso 1 1 calc R U . . .
O1 O 0.5540(8) 0.0807(16) 0.1791(9) 0.052(4) Uani 1 1 d . . . . .
C3 C 0.5172(9) 0.185(2) 0.1679(12) 0.033(4) Uani 1 1 d . . . . .
C6 C 0.5831(10) 0.427(3) 0.2975(12) 0.048(5) Uani 1 1 d . . . . .
H2 H 0.6200 0.4635 0.3505 0.072 Uiso 1 1 calc R U . . .
H3 H 0.5476 0.5024 0.2721 0.072 Uiso 1 1 calc R U . . .
H4 H 0.6012 0.4040 0.2601 0.072 Uiso 1 1 calc R U . . .
C5 C 0.6123(11) 0.166(3) 0.3617(14) 0.048(5) Uani 1 1 d . . . . .
H5 H 0.6484 0.1777 0.3470 0.072 Uiso 1 1 calc R U . . .
H6 H 0.5925 0.0671 0.3458 0.072 Uiso 1 1 calc R U . . .
H7 H 0.6316 0.1791 0.4218 0.072 Uiso 1 1 calc R U . . .
N4 N 0.3268(7) 0.5272(19) 0.1944(9) 0.036(4) Uani 1 1 d . . . . .
H4A H 0.3347 0.5686 0.1550 0.043 Uiso 1 1 calc R U . . .
H4B H 0.2951 0.4551 0.1694 0.043 Uiso 1 1 calc R U . . .
Ni0 Ni 0.5000 0.2540(4) 0.0000 0.0294(7) Uani 1 2 d S T P . .
O2 O 0.4213(6) 0.4122(18) -0.0506(8) 0.046(4) Uani 1 1 d . . . . .
O3 O 0.4293(6) 0.0835(14) -0.0464(9) 0.042(3) Uani 1 1 d . . . . .
Cl0 Cl 0.5000 0.9382(11) 0.5000 0.0452(13) Uani 1 2 d S T P . .
C8 C 0.2576(10) 0.4649(19) 0.2952(12) 0.036(5) Uani 1 1 d . . . . .
H8 H 0.2682 0.4242 0.3494 0.054 Uiso 1 1 calc R U . . .
H9 H 0.2656 0.3896 0.2629 0.054 Uiso 1 1 calc R U . . .
H10 H 0.2096 0.4953 0.2652 0.054 Uiso 1 1 calc R U . . .
C7 C 0.3013(9) 0.593(2) 0.3071(11) 0.032(4) Uani 1 1 d . . . . .
O4 O 0.1997(7) 0.8039(16) 0.1684(10) 0.051(4) Uani 1 1 d . . . . .
O5 O 0.1987(7) 0.6114(17) 0.0930(9) 0.045(3) Uani 1 1 d . . . . .
C10 C 0.2255(8) 0.696(2) 0.1576(11) 0.035(4) Uani 1 1 d . . . . .
C9 C 0.2974(9) 0.6464(19) 0.2280(11) 0.032(4) Uani 1 1 d . . . . .
H11 H 0.3281 0.7342 0.2426 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.1884(7) 0.3041(15) 0.4463(9) 0.029(3) Uani 0.3 1 d . . P A 1
Cl2 Cl 0.2379(12) 0.446(5) 0.5075(15) 0.049(5) Uani 0.2 1 d . . P B 2
C11 C 0.2825(10) 0.720(2) 0.3521(14) 0.047(5) Uani 1 1 d . . . . .
H12 H 0.2381 0.7627 0.3128 0.071 Uiso 1 1 calc R U . . .
H13 H 0.3174 0.7975 0.3712 0.071 Uiso 1 1 calc R U . . .
H14 H 0.2804 0.6790 0.3998 0.071 Uiso 1 1 calc R U . . .
O8 O 0.0832(11) 0.320(2) 0.2654(13) 0.085(6) Uiso 1 1 d . . . . .
O6 O 0.4130(11) 0.980(2) 0.3045(14) 0.094(7) Uiso 1 1 d . . . . .
O12 O 0.3733(13) -0.387(3) 0.0552(16) 0.111(8) Uiso 1 1 d . . . . .
O9 O 0.2597(12) 0.058(3) 0.2617(15) 0.105(7) Uiso 1 1 d . . . . .
O10 O 0.3265(16) 0.109(4) 0.0761(19) 0.139(10) Uiso 1 1 d . . . . .
O11 O 0.4633(13) -0.258(3) 0.2523(16) 0.109(8) Uiso 1 1 d . . . . .
O13 O 0.2360(17) 0.248(4) 0.126(2) 0.140(12) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N2 Pt1 N3 173.9(6) . .
N2 Pt1 S11 89.5(5) . .
N3 Pt1 S11 93.4(4) . .
N2 Pt1 S9 92.5(5) . .
N3 Pt1 S9 86.4(4) . .
S11 Pt1 S9 162.58(15) . .
N4 Pd0 N0 94.1(6) . .
N4 Pd0 S9 176.3(5) . .
N0 Pd0 S9 83.1(4) . .
N4 Pd0 S11 84.2(4) . 2_656
N0 Pd0 S11 177.3(5) . 2_656
S9 Pd0 S11 98.72(15) . 2_656
C7 S11 Pd0 99.9(6) 2_656 2_656
C7 S11 Pt1 115.8(6) 2_656 .
Pd0 S11 Pt1 114.25(18) 2_656 .
C0 S9 Pd0 99.1(6) . .
C0 S9 Pt1 116.3(6) . .
Pd0 S9 Pt1 114.46(18) . .
Pt1 N3 H3A 109.5 . .
Pt1 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
Pt1 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
N0 C1 C0 109.9(13) . .
N0 C1 C3 111.5(14) . .
C0 C1 C3 110.9(15) . .
N0 C1 H1 108.1 . .
C0 C1 H1 108.1 . .
C3 C1 H1 108.1 . .
C1 N0 Pd0 116.1(10) . .
C1 N0 H0A 108.3 . .
Pd0 N0 H0A 108.3 . .
C1 N0 H0B 108.3 . .
Pd0 N0 H0B 108.3 . .
H0A N0 H0B 107.4 . .
C6 C0 C1 113.8(15) . .
C6 C0 C5 110.7(15) . .
C1 C0 C5 110.4(14) . .
C6 C0 S9 115.4(13) . .
C1 C0 S9 101.0(11) . .
C5 C0 S9 104.8(13) . .
C3 O0 Ni0 127.0(12) . .
Pt1 N2 H2A 109.5 . .
Pt1 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Pt1 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
O1 C3 O0 127.4(18) . .
O1 C3 C1 119.9(17) . .
O0 C3 C1 112.6(16) . .
C0 C6 H2 109.5 . .
C0 C6 H3 109.5 . .
H2 C6 H3 109.5 . .
C0 C6 H4 109.5 . .
H2 C6 H4 109.5 . .
H3 C6 H4 109.5 . .
C0 C5 H5 109.5 . .
C0 C5 H6 109.5 . .
H5 C5 H6 109.5 . .
C0 C5 H7 109.5 . .
H5 C5 H7 109.5 . .
H6 C5 H7 109.5 . .
C9 N4 Pd0 114.1(10) . .
C9 N4 H4A 108.7 . .
Pd0 N4 H4A 108.7 . .
C9 N4 H4B 108.7 . .
Pd0 N4 H4B 108.7 . .
H4A N4 H4B 107.6 . .
O0 Ni0 O0 171.4(7) . 2_655
O0 Ni0 O3 93.9(5) . 2_655
O0 Ni0 O3 92.5(5) 2_655 2_655
O0 Ni0 O3 92.5(5) . .
O0 Ni0 O3 93.9(5) 2_655 .
O3 Ni0 O3 83.9(7) 2_655 .
O0 Ni0 O2 88.3(5) . 2_655
O0 Ni0 O2 85.8(5) 2_655 2_655
O3 Ni0 O2 90.9(6) 2_655 2_655
O3 Ni0 O2 174.8(6) . 2_655
O0 Ni0 O2 85.8(5) . .
O0 Ni0 O2 88.3(5) 2_655 .
O3 Ni0 O2 174.8(6) 2_655 .
O3 Ni0 O2 90.9(6) . .
O2 Ni0 O2 94.3(8) 2_655 .
C7 C8 H8 109.5 . .
C7 C8 H9 109.5 . .
H8 C8 H9 109.5 . .
C7 C8 H10 109.5 . .
H8 C8 H10 109.5 . .
H9 C8 H10 109.5 . .
C8 C7 C9 113.2(16) . .
C8 C7 C11 108.8(16) . .
C9 C7 C11 111.7(16) . .
C8 C7 S11 115.2(13) . 2_656
C9 C7 S11 102.1(12) . 2_656
C11 C7 S11 105.5(12) . 2_656
O4 C10 O5 126.3(17) . .
O4 C10 C9 119.0(18) . .
O5 C10 C9 114.7(17) . .
C7 C9 N4 109.5(14) . .
C7 C9 C10 116.4(15) . .
N4 C9 C10 109.9(15) . .
C7 C9 H11 106.9 . .
N4 C9 H11 106.9 . .
C10 C9 H11 106.9 . .
C7 C11 H12 109.5 . .
C7 C11 H13 109.5 . .
H12 C11 H13 109.5 . .
C7 C11 H14 109.5 . .
H12 C11 H14 109.5 . .
H13 C11 H14 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N2 2.055(13) .
Pt1 N3 2.060(14) .
Pt1 S11 2.313(4) .
Pt1 S9 2.317(4) .
Pd0 N4 2.058(14) .
Pd0 N0 2.092(15) .
Pd0 S9 2.268(4) .
Pd0 S11 2.271(4) 2_656
S11 C7 1.852(18) 2_656
S11 Pd0 2.271(4) 2_656
S9 C0 1.859(17) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N3 H3C 0.9100 .
C1 N0 1.47(2) .
C1 C0 1.55(2) .
C1 C3 1.56(2) .
C1 H1 1.0000 .
N0 H0A 0.9100 .
N0 H0B 0.9100 .
C0 C6 1.51(3) .
C0 C5 1.63(2) .
O0 C3 1.26(2) .
O0 Ni0 2.064(12) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 H2C 0.9100 .
O1 C3 1.21(2) .
C6 H2 0.9800 .
C6 H3 0.9800 .
C6 H4 0.9800 .
C5 H5 0.9800 .
C5 H6 0.9800 .
C5 H7 0.9800 .
N4 C9 1.55(2) .
N4 H4A 0.9100 .
N4 H4B 0.9100 .
Ni0 O0 2.064(12) 2_655
Ni0 O3 2.079(12) 2_655
Ni0 O3 2.079(12) .
Ni0 O2 2.108(14) 2_655
Ni0 O2 2.108(14) .
C8 C7 1.47(3) .
C8 H8 0.9800 .
C8 H9 0.9800 .
C8 H10 0.9800 .
C7 C9 1.50(3) .
C7 C11 1.59(3) .
C7 S11 1.852(18) 2_656
O4 C10 1.20(2) .
O5 C10 1.29(2) .
C10 C9 1.57(2) .
C9 H11 1.0000 .
C11 H12 0.9800 .
C11 H13 0.9800 .
C11 H14 0.9800 .
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
_geom_torsion_site_symmetry_1
C0 C1 N0 Pd0 -39.3(19) .
C3 C1 N0 Pd0 -162.7(12) .
N0 C1 C0 C6 -66(2) .
C3 C1 C0 C6 58(2) .
N0 C1 C0 C5 168.8(15) .
C3 C1 C0 C5 -67.4(19) .
N0 C1 C0 S9 58.3(15) .
C3 C1 C0 S9 -177.9(12) .
Pd0 S9 C0 C6 73.5(13) .
Pt1 S9 C0 C6 -49.7(14) .
Pd0 S9 C0 C1 -49.8(10) .
Pt1 S9 C0 C1 -172.9(8) .
Pd0 S9 C0 C5 -164.5(11) .
Pt1 S9 C0 C5 72.4(12) .
Ni0 O0 C3 O1 5(3) .
Ni0 O0 C3 C1 -173.1(11) .
N0 C1 C3 O1 -163.8(18) .
C0 C1 C3 O1 73(2) .
N0 C1 C3 O0 15(2) .
C0 C1 C3 O0 -108.3(17) .
C8 C7 C9 N4 -65.6(19) .
C11 C7 C9 N4 171.2(14) .
S11 C7 C9 N4 58.8(15) 2_656
C8 C7 C9 C10 60(2) .
C11 C7 C9 C10 -63(2) .
S11 C7 C9 C10 -175.8(13) 2_656
Pd0 N4 C9 C7 -43.7(17) .
Pd0 N4 C9 C10 -172.7(12) .
O4 C10 C9 C7 66(2) .
O5 C10 C9 C7 -111.5(19) .
O4 C10 C9 N4 -168.5(18) .
O5 C10 C9 N4 14(2) .
