#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/78/2017821.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_2017821
loop_
_publ_author_name
'Schmitt, Laurette'
'Labat, Gaël'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Crystal-to-crystal transformation upon dehydration of a copper(II)
 2,2':6',2''-terpyridine complex
;
_journal_coeditor_code           GA3158
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m343
_journal_page_last               m347
_journal_paper_doi               10.1107/S0108270110041090
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu2 (C15 H11 N3)2 (Cl)2 (S2 O6)] , H2 O'
_chemical_formula_moiety         'C30 H22 Cl2 Cu2 N6 O6 S2, (H2 O)'
_chemical_formula_sum            'C30 H24 Cl2 Cu2 N6 O7 S2'
_chemical_formula_weight         842.65
_chemical_name_systematic
;
(μ-dithionato-1:2κ²O:O')-bis[2,2':6',2''-terpyridyl-κ³N,N',N'')\
copper(II)] monohydrate
;
_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           SHELXL97
_cell_angle_alpha                107.927(13)
_cell_angle_beta                 99.171(13)
_cell_angle_gamma                105.244(13)
_cell_formula_units_Z            1
_cell_length_a                   8.1961(13)
_cell_length_b                   8.6029(15)
_cell_length_c                   12.2566(19)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      1.81
_cell_volume                     765.7(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2006)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'φ and ω 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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.8455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2724
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                2001
_reflns_number_total             2724
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ga3158.cif
_cod_data_source_block           II
_cod_database_code               2017821
_cod_database_fobs_code          2017821
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu1 0.62148(6) 0.64301(5) 0.16282(4) 0.0323(2) Uani . . 1.000
Cl Cl1 0.73281(12) 0.69647(12) 0.01910(8) 0.0389(3) Uani . . 1.000
S S1 0.89632(11) 0.87944(11) 0.44994(7) 0.0329(3) Uani . . 1.000
O O1 0.8512(3) 0.8817(3) 0.33023(19) 0.0366(8) Uani . . 1.000
O O2 0.7588(3) 0.8854(3) 0.5098(2) 0.0404(8) Uani . . 1.000
O O3 0.9735(3) 0.7477(3) 0.4565(2) 0.0411(9) Uani . . 1.000
N N1 0.4520(4) 0.7782(3) 0.1677(2) 0.0330(9) Uani . . 1.000
N N2 0.4891(4) 0.5609(3) 0.2630(2) 0.0301(9) Uani . . 1.000
N N3 0.7276(4) 0.4603(3) 0.1821(2) 0.0330(9) Uani . . 1.000
C C1 0.4386(5) 0.8893(4) 0.1132(3) 0.0370(11) Uani . . 1.000
C C2 0.3136(5) 0.9691(5) 0.1192(3) 0.0389(12) Uani . . 1.000
C C3 0.1949(5) 0.9339(4) 0.1827(3) 0.0416(12) Uani . . 1.000
C C4 0.2074(5) 0.8198(4) 0.2414(3) 0.0366(11) Uani . . 1.000
C C5 0.3368(4) 0.7473(4) 0.2330(3) 0.0322(10) Uani . . 1.000
C C6 0.3602(4) 0.6214(4) 0.2890(3) 0.0326(11) Uani . . 1.000
C C7 0.2589(5) 0.5621(5) 0.3576(3) 0.0384(11) Uani . . 1.000
C C8 0.2891(5) 0.4308(5) 0.3924(3) 0.0364(11) Uani . . 1.000
C C9 0.4191(5) 0.3654(5) 0.3618(3) 0.0370(12) Uani . . 1.000
C C10 0.5217(4) 0.4362(4) 0.2975(3) 0.0330(11) Uani . . 1.000
C C11 0.6644(4) 0.3830(4) 0.2556(3) 0.0339(11) Uani . . 1.000
C C12 0.7306(5) 0.2649(4) 0.2849(3) 0.0379(11) Uani . . 1.000
C C13 0.8586(5) 0.2186(5) 0.2354(3) 0.0429(12) Uani . . 1.000
C C14 0.9197(5) 0.2937(5) 0.1585(3) 0.0412(12) Uani . . 1.000
C C15 0.8518(5) 0.4142(4) 0.1351(3) 0.0369(12) Uani . . 1.000
O O1W 0.5551(7) 0.0699(7) 0.4479(5) 0.051(2) Uani . . 0.500
H H1 0.51940 0.91410 0.06820 0.0440 Uiso calc R 1.000
H H2 0.30960 1.04780 0.07960 0.0470 Uiso calc R 1.000
H H3 0.10600 0.98590 0.18680 0.0500 Uiso calc R 1.000
H H4 0.12720 0.79320 0.28640 0.0440 Uiso calc R 1.000
H H7 0.17170 0.60960 0.38010 0.0460 Uiso calc R 1.000
H H8 0.21950 0.38550 0.43770 0.0440 Uiso calc R 1.000
H H9 0.43810 0.27390 0.38420 0.0440 Uiso calc R 1.000
H H12 0.68820 0.21590 0.33880 0.0460 Uiso calc R 1.000
H H13 0.90410 0.13620 0.25380 0.0520 Uiso calc R 1.000
H H14 1.00690 0.26300 0.12250 0.0500 Uiso calc R 1.000
H H15 0.89540 0.46680 0.08320 0.0440 Uiso calc R 1.000
H H1WA 0.472(9) 0.065(13) 0.486(8) 0.0750 Uiso . . 0.500
H H1WB 0.638(9) 0.044(13) 0.487(8) 0.0750 Uiso . . 0.500
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Cu1 O1 . . . 96.47(7) no
Cl1 Cu1 N1 . . . 99.26(8) no
Cl1 Cu1 N2 . . . 168.94(8) no
Cl1 Cu1 N3 . . . 99.51(9) no
O1 Cu1 N1 . . . 93.04(10) no
O1 Cu1 N2 . . . 94.58(10) no
O1 Cu1 N3 . . . 93.51(10) no
N1 Cu1 N2 . . . 79.90(12) no
N1 Cu1 N3 . . . 159.27(12) no
N2 Cu1 N3 . . . 79.99(12) no
O1 S1 O2 . . . 113.74(15) no
O1 S1 O3 . . . 113.51(15) no
S1 S1 O1 2_776 . . 104.69(12) no
O2 S1 O3 . . . 114.28(16) no
S1 S1 O2 2_776 . . 104.64(11) no
S1 S1 O3 2_776 . . 104.57(11) no
Cu1 O1 S1 . . . 123.60(15) no
H1WA O1W H1WB . . . 107(8) no
Cu1 N1 C1 . . . 128.2(3) no
C1 N1 C5 . . . 117.2(3) no
Cu1 N1 C5 . . . 114.6(2) no
Cu1 N2 C6 . . . 119.1(2) no
Cu1 N2 C10 . . . 118.8(3) no
C6 N2 C10 . . . 121.9(3) no
Cu1 N3 C11 . . . 113.8(2) no
Cu1 N3 C15 . . . 127.9(2) no
C11 N3 C15 . . . 118.2(3) no
N1 C1 C2 . . . 123.2(4) no
C1 C2 C3 . . . 119.3(4) no
C2 C3 C4 . . . 118.6(4) no
C3 C4 C5 . . . 118.9(4) no
N1 C5 C6 . . . 113.5(3) no
C4 C5 C6 . . . 123.7(3) no
N1 C5 C4 . . . 122.8(3) no
N2 C6 C7 . . . 120.9(3) no
C5 C6 C7 . . . 126.1(3) no
N2 C6 C5 . . . 112.9(3) no
C6 C7 C8 . . . 117.8(4) no
C7 C8 C9 . . . 120.7(4) no
C8 C9 C10 . . . 118.6(4) no
N2 C10 C9 . . . 119.9(3) no
C9 C10 C11 . . . 126.7(3) no
N2 C10 C11 . . . 113.3(3) no
N3 C11 C12 . . . 121.4(3) no
C10 C11 C12 . . . 124.8(3) no
N3 C11 C10 . . . 113.8(3) no
C11 C12 C13 . . . 119.6(3) no
C12 C13 C14 . . . 119.0(4) no
C13 C14 C15 . . . 118.7(4) no
N3 C15 C14 . . . 123.0(3) no
C2 C1 H1 . . . 118.00 no
N1 C1 H1 . . . 118.00 no
C1 C2 H2 . . . 120.00 no
C3 C2 H2 . . . 120.00 no
C4 C3 H3 . . . 121.00 no
C2 C3 H3 . . . 121.00 no
C3 C4 H4 . . . 120.00 no
C5 C4 H4 . . . 121.00 no
C8 C7 H7 . . . 121.00 no
C6 C7 H7 . . . 121.00 no
C7 C8 H8 . . . 120.00 no
C9 C8 H8 . . . 120.00 no
C10 C9 H9 . . . 121.00 no
C8 C9 H9 . . . 121.00 no
C11 C12 H12 . . . 120.00 no
C13 C12 H12 . . . 120.00 no
C14 C13 H13 . . . 120.00 no
C12 C13 H13 . . . 120.00 no
C13 C14 H14 . . . 121.00 no
C15 C14 H14 . . . 121.00 no
N3 C15 H15 . . . 119.00 no
C14 C15 H15 . . . 118.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 Cl1 . . 2.2220(11) yes
Cu1 O1 . . 2.473(2) yes
Cu1 N1 . . 2.030(3) yes
Cu1 N2 . . 1.934(3) yes
Cu1 N3 . . 2.041(3) yes
S1 O1 . . 1.462(2) no
S1 O2 . . 1.443(3) no
S1 O3 . . 1.452(3) no
S1 S1 . 2_776 2.1474(13) no
O1W H1WA . . 0.88(8) no
O1W H1WB . . 0.89(9) no
N1 C5 . . 1.357(5) no
N1 C1 . . 1.340(4) no
N2 C6 . . 1.335(5) no
N2 C10 . . 1.340(4) no
N3 C15 . . 1.336(5) no
N3 C11 . . 1.363(4) no
C1 C2 . . 1.375(6) no
C2 C3 . . 1.370(6) no
C3 C4 . . 1.399(5) no
C4 C5 . . 1.367(5) no
C5 C6 . . 1.485(5) no
C6 C7 . . 1.386(5) no
C7 C8 . . 1.389(6) no
C8 C9 . . 1.380(6) no
C9 C10 . . 1.392(5) no
C10 C11 . . 1.473(5) no
C11 C12 . . 1.381(5) no
C12 C13 . . 1.379(6) no
C13 C14 . . 1.383(6) no
C14 C15 . . 1.379(6) no
C1 H1 . . 0.9500 no
C2 H2 . . 0.9500 no
C3 H3 . . 0.9500 no
C4 H4 . . 0.9500 no
C7 H7 . . 0.9500 no
C8 H8 . . 0.9500 no
C9 H9 . . 0.9500 no
C12 H12 . . 0.9500 no
C13 H13 . . 0.9500 no
C14 H14 . . 0.9500 no
C15 H15 . . 0.9500 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cu1 Cl1 3.3765(12) . 2_665 yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1WA O2 2_666 0.88(8) 2.05(8) 2.803(7) 142(8) yes
O1W H1WB O2 1_545 0.89(9) 1.94(10) 2.759(7) 153(10) yes
C7 H7 O3 1_455 0.95 2.40 3.342(5) 174 yes
C8 H8 O3 2_666 0.95 2.47 3.421(5) 176 yes
C9 H9 O1W . 0.95 2.47 3.404(7) 168 yes
C12 H12 O1W . 0.95 2.31 3.253(7) 172 yes
C13 H13 O1 1_545 0.95 2.60 3.429(5) 146 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl1 Cu1 O1 S1 . . . . -154.20(16) no
N1 Cu1 O1 S1 . . . . 106.12(18) no
N2 Cu1 O1 S1 . . . . 26.02(19) no
N3 Cu1 O1 S1 . . . . -54.21(19) no
Cl1 Cu1 N1 C1 . . . . -10.0(3) no
Cl1 Cu1 N1 C5 . . . . 168.5(2) no
O1 Cu1 N1 C1 . . . . 87.0(3) no
O1 Cu1 N1 C5 . . . . -94.4(2) no
N2 Cu1 N1 C1 . . . . -178.9(3) no
N2 Cu1 N1 C5 . . . . -0.3(2) no
N3 Cu1 N1 C1 . . . . -164.7(3) no
N3 Cu1 N1 C5 . . . . 13.8(4) no
O1 Cu1 N2 C6 . . . . 92.1(2) no
O1 Cu1 N2 C10 . . . . -92.4(2) no
N1 Cu1 N2 C6 . . . . -0.2(2) no
N1 Cu1 N2 C10 . . . . 175.3(3) no
N3 Cu1 N2 C6 . . . . -175.1(3) no
N3 Cu1 N2 C10 . . . . 0.4(2) no
Cl1 Cu1 N3 C11 . . . . -171.9(2) no
Cl1 Cu1 N3 C15 . . . . 10.4(3) no
O1 Cu1 N3 C11 . . . . 90.9(2) no
O1 Cu1 N3 C15 . . . . -86.8(3) no
N1 Cu1 N3 C11 . . . . -17.3(4) no
N1 Cu1 N3 C15 . . . . 165.0(3) no
N2 Cu1 N3 C11 . . . . -3.1(2) no
N2 Cu1 N3 C15 . . . . 179.2(3) no
O2 S1 O1 Cu1 . . . . -66.8(2) no
O3 S1 O1 Cu1 . . . . 66.1(2) no
S1 S1 O1 Cu1 2_776 . . . 179.55(12) no
O1 S1 S1 O1 . . 2_776 2_776 -180.00(15) no
O1 S1 S1 O2 . . 2_776 2_776 -60.09(16) no
O1 S1 S1 O3 . . 2_776 2_776 60.38(16) no
O2 S1 S1 O1 . . 2_776 2_776 60.09(16) no
O2 S1 S1 O2 . . 2_776 2_776 180.00(16) no
O2 S1 S1 O3 . . 2_776 2_776 -59.54(16) no
O3 S1 S1 O1 . . 2_776 2_776 -60.38(16) no
O3 S1 S1 O2 . . 2_776 2_776 59.54(16) no
O3 S1 S1 O3 . . 2_776 2_776 -180.00(15) no
Cu1 N1 C1 C2 . . . . 177.4(3) no
C5 N1 C1 C2 . . . . -1.1(5) no
Cu1 N1 C5 C4 . . . . -176.6(3) no
Cu1 N1 C5 C6 . . . . 0.7(4) no
C1 N1 C5 C4 . . . . 2.2(5) no
C1 N1 C5 C6 . . . . 179.4(3) no
Cu1 N2 C6 C5 . . . . 0.6(4) no
Cu1 N2 C6 C7 . . . . 178.1(3) no
C10 N2 C6 C5 . . . . -174.8(3) no
C10 N2 C6 C7 . . . . 2.8(5) no
Cu1 N2 C10 C9 . . . . -175.0(3) no
Cu1 N2 C10 C11 . . . . 2.3(4) no
C6 N2 C10 C9 . . . . 0.4(5) no
C6 N2 C10 C11 . . . . 177.6(3) no
Cu1 N3 C11 C10 . . . . 5.1(4) no
Cu1 N3 C11 C12 . . . . -175.6(3) no
C15 N3 C11 C10 . . . . -177.0(3) no
C15 N3 C11 C12 . . . . 2.4(5) no
Cu1 N3 C15 C14 . . . . 177.0(3) no
C11 N3 C15 C14 . . . . -0.7(5) no
N1 C1 C2 C3 . . . . -0.6(6) no
C1 C2 C3 C4 . . . . 1.2(5) no
C2 C3 C4 C5 . . . . -0.2(5) no
C3 C4 C5 N1 . . . . -1.5(5) no
C3 C4 C5 C6 . . . . -178.5(3) no
N1 C5 C6 N2 . . . . -0.8(4) no
N1 C5 C6 C7 . . . . -178.2(3) no
C4 C5 C6 N2 . . . . 176.4(3) no
C4 C5 C6 C7 . . . . -1.0(6) no
N2 C6 C7 C8 . . . . -3.7(5) no
C5 C6 C7 C8 . . . . 173.5(3) no
C6 C7 C8 C9 . . . . 1.6(5) no
C7 C8 C9 C10 . . . . 1.3(5) no
C8 C9 C10 N2 . . . . -2.4(5) no
C8 C9 C10 C11 . . . . -179.2(3) no
N2 C10 C11 N3 . . . . -4.8(4) no
N2 C10 C11 C12 . . . . 175.8(3) no
C9 C10 C11 N3 . . . . 172.2(3) no
C9 C10 C11 C12 . . . . -7.1(6) no
N3 C11 C12 C13 . . . . -2.6(5) no
C10 C11 C12 C13 . . . . 176.7(3) no
C11 C12 C13 C14 . . . . 0.9(5) no
C12 C13 C14 C15 . . . . 0.8(6) no
C13 C14 C15 N3 . . . . -0.9(6) no
