#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:34:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180440 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/09/7210930.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_7210930
loop_
_publ_author_name
'Zeisler, Christoph'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 A new synthetic approach to force bond formation between a transition
 metal complex and a thiostannate anion: solvothermal synthesis and
 crystal structure of [Co2(cyclam)2Sn2S6]·2H2O
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8874
_journal_paper_doi               10.1039/c3ce40976g
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C20 H52 Co2 N8 O2 S6 Sn2'
_chemical_formula_weight         984.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.769(6)
_cell_angle_beta                 94.398(6)
_cell_angle_gamma                102.954(6)
_cell_formula_units_Z            1
_cell_length_a                   9.0686(6)
_cell_length_b                   9.8673(7)
_cell_length_c                   10.1779(8)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     876.36(11)
_computing_cell_refinement       'X-Area, STOE & CIE'
_computing_data_collection       'X-Area, STOE & CIE'
_computing_data_reduction        'X-Area, STOE & CIE'
_computing_molecular_graphics    'XP and Diamond'
_computing_publication_material  SHELXTL-PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9924
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and S-Shale from STOE'
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0029(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0257P)²+0.2151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                3631
_reflns_number_total             4210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40976g.txt
_cod_data_source_block           cz54b
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.36720(2) 0.883389(19) 0.561845(17) 0.02167(6) Uani 1 1 d .
S1 S 0.40703(9) 0.81694(7) 0.77238(7) 0.03209(17) Uani 1 1 d .
S2 S 0.13034(8) 0.77117(8) 0.44659(7) 0.03113(16) Uani 1 1 d .
S3 S 0.42063(8) 1.13860(7) 0.56892(7) 0.02841(14) Uani 1 1 d .
Co1 Co 0.5000 1.0000 1.0000 0.02307(11) Uani 1 2 d S
N1 N 0.5328(3) 1.1620(2) 0.8987(2) 0.0294(5) Uani 1 1 d .
H1N H 0.4972 1.1252 0.8129 0.035 Uiso 1 1 calc R
C1 C 0.6983(4) 1.2152(3) 0.8982(3) 0.0399(7) Uani 1 1 d .
H1A H 0.7403 1.2766 0.9804 0.048 Uiso 1 1 calc R
H1B H 0.7186 1.2684 0.8246 0.048 Uiso 1 1 calc R
C2 C 0.7696(4) 1.0931(4) 0.8845(3) 0.0415(8) Uani 1 1 d .
H2A H 0.8796 1.1254 0.8956 0.050 Uiso 1 1 calc R
H2B H 0.7390 1.0391 0.7968 0.050 Uiso 1 1 calc R
N2 N 0.7186(3) 1.0046(3) 0.9887(2) 0.0314(5) Uani 1 1 d .
H2N H 0.7693 1.0517 1.0674 0.038 Uiso 1 1 calc R
C3 C 0.7647(4) 0.8700(4) 0.9681(4) 0.0458(8) Uani 1 1 d .
H3A H 0.8744 0.8883 0.9687 0.055 Uiso 1 1 calc R
H3B H 0.7194 0.8192 0.8817 0.055 Uiso 1 1 calc R
C4 C 0.7156(5) 0.7803(4) 1.0752(4) 0.0505(9) Uani 1 1 d .
H4A H 0.7634 0.7015 1.0677 0.061 Uiso 1 1 calc R
H4B H 0.7520 0.8356 1.1616 0.061 Uiso 1 1 calc R
C5 C 0.5454(4) 0.7249(3) 1.0685(3) 0.0428(8) Uani 1 1 d .
H5A H 0.5068 0.6771 0.9796 0.051 Uiso 1 1 calc R
H5B H 0.5235 0.6570 1.1302 0.051 Uiso 1 1 calc R
Co2 Co 0.0000 0.5000 0.5000 0.02281(11) Uani 1 2 d S
N11 N 0.1397(3) 0.5236(2) 0.6644(2) 0.0293(5) Uani 1 1 d .
H11N H 0.1940 0.6144 0.6758 0.035 Uiso 1 1 calc R
C11 C 0.2512(4) 0.4366(3) 0.6386(3) 0.0389(7) Uani 1 1 d .
H11A H 0.2068 0.3395 0.6474 0.047 Uiso 1 1 calc R
H11B H 0.3412 0.4701 0.7020 0.047 Uiso 1 1 calc R
C12 C 0.2923(3) 0.4478(3) 0.5003(4) 0.0384(7) Uani 1 1 d .
H12A H 0.3484 0.5425 0.4943 0.046 Uiso 1 1 calc R
H12B H 0.3555 0.3835 0.4758 0.046 Uiso 1 1 calc R
N12 N 0.1490(3) 0.4119(3) 0.4105(2) 0.0303(5) Uani 1 1 d .
H12N H 0.1127 0.3175 0.4054 0.036 Uiso 1 1 calc R
C13 C 0.1776(4) 0.4396(4) 0.2738(3) 0.0432(8) Uani 1 1 d .
H13A H 0.2469 0.3850 0.2407 0.052 Uiso 1 1 calc R
H13B H 0.2258 0.5381 0.2757 0.052 Uiso 1 1 calc R
C14 C 0.0316(5) 0.4025(4) 0.1802(3) 0.0491(9) Uani 1 1 d .
H14A H 0.0571 0.4066 0.0897 0.059 Uiso 1 1 calc R
H14B H -0.0214 0.3067 0.1857 0.059 Uiso 1 1 calc R
C15 C -0.0743(4) 0.4980(3) 0.2096(3) 0.0402(8) Uani 1 1 d .
H15A H -0.0187 0.5950 0.2149 0.048 Uiso 1 1 calc R
H15B H -0.1558 0.4796 0.1377 0.048 Uiso 1 1 calc R
O1 O -0.0053(5) 0.9475(5) 0.6897(4) 0.0958(13) Uani 1 1 d .
H1O H 0.0196 0.9113 0.6207 0.144 Uiso 1 1 d R
H2O H 0.0070 1.0322 0.6880 0.144 Uiso 1 1 d R
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
S2 Sn1 S1 113.92(3) . .
S2 Sn1 S3 112.29(3) . .
S1 Sn1 S3 112.25(2) . .
S2 Sn1 S3 112.63(3) . 2_676
S1 Sn1 S3 110.82(3) . 2_676
S3 Sn1 S3 93.21(2) . 2_676
Sn1 S1 Co1 124.34(3) . .
Sn1 S3 Sn1 86.79(2) . 2_676
N1 Co1 N1 180.000(1) 2_677 .
N1 Co1 N2 86.31(11) 2_677 2_677
N1 Co1 N2 93.69(11) . 2_677
N1 Co1 N2 93.69(11) 2_677 .
N1 Co1 N2 86.31(11) . .
N2 Co1 N2 180.000(1) 2_677 .
N1 Co1 S1 91.32(7) 2_677 2_677
N1 Co1 S1 88.68(7) . 2_677
N2 Co1 S1 93.65(7) 2_677 2_677
N2 Co1 S1 86.35(7) . 2_677
N1 Co1 S1 88.68(7) 2_677 .
N1 Co1 S1 91.32(7) . .
N2 Co1 S1 86.35(7) 2_677 .
N2 Co1 S1 93.65(7) . .
S1 Co1 S1 180.000(1) 2_677 .
C5 N1 C1 112.5(3) 2_677 .
C5 N1 Co1 119.1(2) 2_677 .
C1 N1 Co1 107.91(18) . .
N1 C1 C2 108.4(2) . .
C1 C2 N2 108.0(3) . .
C3 N2 C2 111.1(3) . .
C3 N2 Co1 118.5(2) . .
C2 N2 Co1 107.09(19) . .
N2 C3 C4 111.4(3) . .
C5 C4 C3 113.9(3) . .
N1 C5 C4 111.8(3) 2_677 .
N11 Co2 N11 180.000(1) . 2_566
N11 Co2 N12 86.00(10) . .
N11 Co2 N12 94.00(10) 2_566 .
N11 Co2 N12 94.00(10) . 2_566
N11 Co2 N12 86.00(10) 2_566 2_566
N12 Co2 N12 180.000(1) . 2_566
C15 N11 C11 111.7(2) 2_566 .
C15 N11 Co2 118.6(2) 2_566 .
C11 N11 Co2 107.93(19) . .
N11 C11 C12 107.8(2) . .
N12 C12 C11 107.5(2) . .
C12 N12 C13 111.1(3) . .
C12 N12 Co2 107.67(19) . .
C13 N12 Co2 118.4(2) . .
N12 C13 C14 111.8(3) . .
C15 C14 C13 113.7(3) . .
N11 C15 C14 111.3(3) 2_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 S2 2.3360(7) .
Sn1 S1 2.3390(7) .
Sn1 S3 2.4467(7) .
Sn1 S3 2.4561(8) 2_676
S1 Co1 2.7151(7) .
S3 Sn1 2.4561(8) 2_676
Co1 N1 1.982(2) 2_677
Co1 N1 1.982(2) .
Co1 N2 1.986(2) 2_677
Co1 N2 1.986(2) .
Co1 S1 2.7151(7) 2_677
N1 C5 1.471(4) 2_677
N1 C1 1.475(4) .
C1 C2 1.487(5) .
C2 N2 1.488(4) .
N2 C3 1.477(4) .
C3 C4 1.515(5) .
C4 C5 1.511(6) .
C5 N1 1.471(4) 2_677
Co2 N11 1.977(2) .
Co2 N11 1.977(2) 2_566
Co2 N12 1.985(2) .
Co2 N12 1.985(2) 2_566
N11 C15 1.471(4) 2_566
N11 C11 1.485(4) .
C11 C12 1.493(5) .
C12 N12 1.478(4) .
N12 C13 1.481(4) .
C13 C14 1.517(5) .
C14 C15 1.511(5) .
C15 N11 1.471(4) 2_566
