#------------------------------------------------------------------------------
#$Date: 2016-05-06 04:26:21 +0300 (Fri, 06 May 2016) $
#$Revision: 182700 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/86/7038673.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_7038673
loop_
_publ_author_name
'Delgado, Esther'
'Gómez-García, Carlos J'
'Hernández, Diego'
'Hernández, Elisa'
'Martín, Avelino'
'Zamora, Félix'
_publ_section_title
;
 Unprecedented layered coordination polymers of dithiolene group 10
 metals: magnetic and electrical properties.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6696
_journal_page_last               6701
_journal_paper_doi               10.1039/c6dt00464d
_journal_volume                  45
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 Cl4 K2 Ni1 O5 S4'
_chemical_formula_sum            'C24 H32 Cl4 K2 Ni O5 S4'
_chemical_formula_weight         807.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2015-01-28T11:51:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.273(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.064(3)
_cell_length_b                   14.446(5)
_cell_length_c                   26.473(4)
_cell_measurement_reflns_used    152
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3438.4(17)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Diamond (Branderburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26810
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.331
_refine_diff_density_min         -1
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.124
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0865P)²+32.0534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0
_reflns_number_gt                2567
_reflns_number_total             3952
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt00464d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7038673--7038676.cif.'
_cod_original_cell_volume        3438.5(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C24 H32 Cl4 K2 Ni1 O5 S4'
_cod_database_code               7038673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.5593(7) 0.9372(5) 0.3661(2) 0.0383(15) Uani 1 1 d . . .
C2 C 0.5840(9) 0.9827(6) 0.4122(3) 0.0483(18) Uani 1 1 d . . .
C3 C 0.6120(9) 0.9372(6) 0.4586(3) 0.055(2) Uani 1 1 d . . .
H3 H 0.6278 0.971 0.4896 0.066 Uiso 1 1 calc R U .
C4 C 0.6164(10) 0.8420(7) 0.4587(3) 0.058(2) Uani 1 1 d . . .
H4 H 0.6339 0.8093 0.49 0.069 Uiso 1 1 calc R U .
C5 C 0.5955(8) 0.7938(5) 0.4132(3) 0.0441(17) Uani 1 1 d . . .
C6 C 0.5635(7) 0.8410(5) 0.3658(2) 0.0358(15) Uani 1 1 d . . .
C51 C -0.0258(16) 0.9394(11) 0.4134(6) 0.124(3) Uani 1 1 d . . .
H51A H -0.1155 0.9276 0.3888 0.148 Uiso 1 1 calc R U .
H51B H -0.0416 0.9962 0.4329 0.148 Uiso 1 1 calc R U .
C52 C 0.0066(16) 0.8623(11) 0.4465(6) 0.124(3) Uani 1 1 d . . .
H52A H -0.0325 0.8745 0.4791 0.148 Uiso 1 1 calc R U .
H52B H -0.0443 0.8067 0.4309 0.148 Uiso 1 1 calc R U .
C53 C 0.1515(16) 0.8460(11) 0.4555(6) 0.124(3) Uani 1 1 d . . .
H53A H 0.1714 0.7789 0.4601 0.148 Uiso 1 1 calc R U .
H53B H 0.1965 0.8793 0.4864 0.148 Uiso 1 1 calc R U .
C54 C 0.2094(17) 0.8805(11) 0.4104(6) 0.124(3) Uani 1 1 d . . .
H54A H 0.3077 0.9099 0.4197 0.148 Uiso 1 1 calc R U .
H54B H 0.22 0.8295 0.3862 0.148 Uiso 1 1 calc R U .
C61 C 0.0965(12) 0.8522(8) 0.2249(5) 0.094(4) Uani 1 1 d . . .
H61A H 0.082 0.8642 0.1877 0.113 Uiso 1 1 calc R U .
H61B H 0.2017 0.8649 0.238 0.113 Uiso 1 1 calc R U .
C62 C 0.0611(17) 0.7598(8) 0.2346(8) 0.151(8) Uani 1 1 d . . .
H62A H 0.1487 0.728 0.2529 0.181 Uiso 1 1 calc R U .
H62B H 0.0313 0.7267 0.2021 0.181 Uiso 1 1 calc R U .
O1 O -0.1510(6) 1.0875(4) 0.2948(2) 0.0601(16) Uani 1 1 d . . .
H1A H -0.2101 1.043 0.3124 0.072 Uiso 1 1 calc R U .
H1B H -0.1767 1.1521 0.3025 0.072 Uiso 1 1 calc R U .
O5 O 0.1021(8) 0.9474(5) 0.3883(3) 0.087(2) Uani 1 1 d . . .
O6 O 0 0.9113(6) 0.25 0.068(3) Uani 1 2 d S T P
S1 S 0.51873(18) 0.99596(12) 0.30775(6) 0.0345(4) Uani 1 1 d . . .
S2 S 0.53309(19) 0.78063(12) 0.30788(6) 0.0369(4) Uani 1 1 d . . .
Cl1 Cl 0.5759(4) 1.10337(16) 0.41364(9) 0.0785(8) Uani 1 1 d . . .
Cl2 Cl 0.6027(3) 0.67318(15) 0.41423(8) 0.0697(7) Uani 1 1 d . . .
K1 K 0.15292(19) 1.05159(13) 0.30830(7) 0.0546(5) Uani 1 1 d . . .
Ni1 Ni 0.5 0.88815(8) 0.25 0.0294(3) Uani 1 2 d S T P
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 0 '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'
S S 0.1246 0.1234 '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'
K K 0.2009 0.2494 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 3 -7 0.203
-7 6 -6 0.187
5 -2 1 0.15
1 -6 10 0.127
0 0 -1 0.12
0 0 1 0.044
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
C2 C1 C6 118.6(7) . .
C2 C1 S1 122.6(6) . .
C6 C1 S1 118.8(5) . .
C1 C2 C3 123.2(8) . .
C1 C2 Cl1 119.5(6) . .
C3 C2 Cl1 117.3(6) . .
C4 C3 C2 118.5(7) . .
C4 C3 H3 120.7 . .
C2 C3 H3 120.7 . .
C3 C4 C5 120.1(7) . .
C3 C4 H4 120 . .
C5 C4 H4 120 . .
C4 C5 C6 121.1(7) . .
C4 C5 Cl2 119.2(6) . .
C6 C5 Cl2 119.7(5) . .
C1 C6 C5 118.5(6) . .
C1 C6 S2 120.0(5) . .
C5 C6 S2 121.5(6) . .
O5 C51 C52 103.7(11) . .
O5 C51 H51A 111 . .
C52 C51 H51A 111 . .
O5 C51 H51B 111 . .
C52 C51 H51B 111 . .
H51A C51 H51B 109 . .
C53 C52 C51 111.9(14) . .
C53 C52 H52A 109.2 . .
C51 C52 H52A 109.2 . .
C53 C52 H52B 109.2 . .
C51 C52 H52B 109.2 . .
H52A C52 H52B 107.9 . .
C52 C53 C54 104.0(14) . .
C52 C53 H53A 110.9 . .
C54 C53 H53A 110.9 . .
C52 C53 H53B 110.9 . .
C54 C53 H53B 110.9 . .
H53A C53 H53B 109 . .
O5 C54 C53 105.7(11) . .
O5 C54 H54A 110.6 . .
C53 C54 H54A 110.6 . .
O5 C54 H54B 110.6 . .
C53 C54 H54B 110.6 . .
H54A C54 H54B 108.7 . .
C62 C61 O6 108.2(10) . .
C62 C61 H61A 110.1 . .
O6 C61 H61A 110.1 . .
C62 C61 H61B 110.1 . .
O6 C61 H61B 110.1 . .
H61A C61 H61B 108.4 . .
C61 C62 C62 108.1(7) . 2
C61 C62 H62A 110.1 . .
C62 C62 H62A 110.1 2 .
C61 C62 H62B 110.1 . .
C62 C62 H62B 110.1 2 .
H62A C62 H62B 108.4 . .
K1 O1 K1 88.54(16) 2 .
K1 O1 H1A 113.9 2 .
K1 O1 H1A 113.9 . .
K1 O1 H1B 113.9 2 .
K1 O1 H1B 113.9 . .
H1A O1 H1B 111.1 . .
C51 O5 C54 107.7(9) . .
C51 O5 K1 130.6(7) . .
C54 O5 K1 121.5(7) . .
C61 O6 C61 107.5(11) 2 .
C61 O6 K1 117.3(6) 2 .
C61 O6 K1 113.3(5) . .
C61 O6 K1 113.3(5) 2 2
C61 O6 K1 117.3(6) . 2
K1 O6 K1 87.5(2) . 2
C1 S1 Ni1 105.1(2) . .
C1 S1 K1 101.8(2) . .
Ni1 S1 K1 100.50(6) . .
C6 S2 Ni1 104.7(2) . .
C6 S2 K1 117.1(2) . 3_545
Ni1 S2 K1 134.09(7) . 3_545
C5 Cl2 K1 120.9(2) . 3_545
O5 K1 O1 154.1(2) . 2
O5 K1 O1 86.5(2) . .
O1 K1 O1 87.48(17) 2 .
O5 K1 O6 84.7(2) . .
O1 K1 O6 69.68(16) 2 .
O1 K1 O6 69.61(14) . .
O5 K1 Cl2 65.37(19) . 3_455
O1 K1 Cl2 137.08(14) 2 3_455
O1 K1 Cl2 77.00(13) . 3_455
O6 K1 Cl2 136.15(8) . 3_455
O5 K1 S1 97.76(16) . .
O1 K1 S1 85.70(12) 2 .
O1 K1 S1 171.94(14) . .
O6 K1 S1 103.90(10) . .
Cl2 K1 S1 110.97(8) 3_455 .
O5 K1 S2 116.78(18) . 3_455
O1 K1 S2 81.74(12) 2 3_455
O1 K1 S2 61.26(12) . 3_455
O6 K1 S2 123.55(13) . 3_455
Cl2 K1 S2 55.63(5) 3_455 3_455
S1 K1 S2 121.77(7) . 3_455
O5 K1 K1 116.81(19) . 2
O1 K1 K1 45.78(13) 2 2
O1 K1 K1 45.68(12) . 2
O6 K1 K1 46.26(12) . 2
Cl2 K1 K1 120.09(8) 3_455 2
S1 K1 K1 126.40(8) . 2
S2 K1 K1 78.83(4) 3_455 2
S1 Ni1 S1 88.48(10) 2_655 .
S1 Ni1 S2 91.42(6) 2_655 2_655
S1 Ni1 S2 176.58(6) . 2_655
S1 Ni1 S2 176.58(6) 2_655 .
S1 Ni1 S2 91.41(6) . .
S2 Ni1 S2 88.89(10) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.382(10) .
C1 C6 1.390(10) .
C1 S1 1.759(7) .
C2 C3 1.387(11) .
C2 Cl1 1.745(8) .
C3 C4 1.376(12) .
C3 H3 0.95 .
C4 C5 1.384(11) .
C4 H4 0.95 .
C5 C6 1.424(9) .
C5 Cl2 1.744(8) .
C6 S2 1.756(7) .
C51 O5 1.413(15) .
C51 C52 1.424(19) .
C51 H51A 0.99 .
C51 H51B 0.99 .
C52 C53 1.326(18) .
C52 H52A 0.99 .
C52 H52B 0.99 .
C53 C54 1.452(18) .
C53 H53A 0.99 .
C53 H53B 0.99 .
C54 O5 1.442(15) .
C54 H54A 0.99 .
C54 H54B 0.99 .
C61 C62 1.404(15) .
C61 O6 1.443(11) .
C61 H61A 0.99 .
C61 H61B 0.99 .
C62 C62 1.46(3) 2
C62 H62A 0.99 .
C62 H62B 0.99 .
O1 K1 2.776(6) 2
O1 K1 2.781(6) .
O1 H1A 0.99 .
O1 H1B 0.99 .
O5 K1 2.684(6) .
O6 C61 1.443(11) 2
O6 K1 2.805(6) .
O6 K1 2.805(6) 2
S1 Ni1 2.1739(19) .
S1 K1 3.414(3) .
S2 Ni1 2.1758(19) .
S2 K1 3.482(3) 3_545
Cl2 K1 3.388(3) 3_545
K1 O1 2.776(6) 2
K1 Cl2 3.388(3) 3_455
K1 S2 3.482(3) 3_455
K1 K1 3.879(4) 2
Ni1 S1 2.1738(19) 2_655
Ni1 S2 2.1758(19) 2_655
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_4
C6 C1 C2 C3 -0.4(11) .
S1 C1 C2 C3 178.2(6) .
C6 C1 C2 Cl1 -178.8(5) .
S1 C1 C2 Cl1 -0.3(9) .
C1 C2 C3 C4 0.4(13) .
Cl1 C2 C3 C4 178.9(7) .
C2 C3 C4 C5 1.0(13) .
C3 C4 C5 C6 -2.4(13) .
C3 C4 C5 Cl2 179.6(7) .
C2 C1 C6 C5 -1.0(10) .
S1 C1 C6 C5 -179.6(5) .
C2 C1 C6 S2 -179.9(5) .
S1 C1 C6 S2 1.5(8) .
C4 C5 C6 C1 2.4(11) .
Cl2 C5 C6 C1 -179.6(5) .
C4 C5 C6 S2 -178.7(6) .
Cl2 C5 C6 S2 -0.8(9) .
O5 C51 C52 C53 21(2) .
C51 C52 C53 C54 -28(2) .
C52 C53 C54 O5 23.0(19) .
O6 C61 C62 C62 1(3) 2
C52 C51 O5 C54 -4.8(17) .
C52 C51 O5 K1 170.1(10) .
C53 C54 O5 C51 -10.8(18) .
C53 C54 O5 K1 173.8(10) .
C62 C61 O6 C61 -0.4(10) 2
C62 C61 O6 K1 130.9(12) .
C62 C61 O6 K1 -129.4(12) 2
C2 C1 S1 Ni1 178.0(5) .
C6 C1 S1 Ni1 -3.4(6) .
C2 C1 S1 K1 -77.5(6) .
C6 C1 S1 K1 101.0(5) .
C1 C6 S2 Ni1 1.2(6) .
C5 C6 S2 Ni1 -177.6(5) .
C1 C6 S2 K1 161.4(5) 3_545
C5 C6 S2 K1 -17.4(6) 3_545
C4 C5 Cl2 K1 -162.2(5) 3_545
C6 C5 Cl2 K1 19.8(7) 3_545
