# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Kay Latham'
_publ_contact_author_email       KAY.LATHAM@RMIT.EDU.AU

_publ_section_title              
;
Synthesis of supramolecular metallo-amine-oxy acid
systems via crystal disassembly/ reassembly
;
loop_
_publ_author_name
'Kay Latham'
'Emily J. Mensforth'
'Colin Rix'
'Jonathan M White'

# Attachment 'new_KL_CrystEngComm_Dec08_X-ray_Data.cif'

#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
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#######################################################################

data_jmwks6a
_database_code_depnum_ccdc_archive 'CCDC 713098'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'iodobis(1,10-phenanthroline)copper(II)
phenylsulphonate dihydrate'
;
_chemical_name_common            
;
'iodobis(1,10-phenanthroline)copper(ii)
                   phenylsulphonate dihydrate'
;
_chemical_melting_point          'decomposes greater than 373K'
_chemical_formula_moiety         'C24 H16 Cu I N4, C6 H3 O3 S, H2 O, O'
_chemical_formula_sum            'C30 H25 Cu I N4 O5 S'
_chemical_formula_weight         744.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c
_symmetry_space_group_Hall       -P2yc

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   23.6321(3)
_cell_length_b                   7.33380(10)
_cell_length_c                   16.9532(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1310(10)
_cell_angle_gamma                90.00
_cell_volume                     2849.30(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    7122
_cell_measurement_theta_min      2.6877
_cell_measurement_theta_max      73.1574

_exptl_crystal_description       'triangular plate'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.5681
_exptl_crystal_size_mid          0.3403
_exptl_crystal_size_min          0.0300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    10.678
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14131
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.86
_diffrn_reflns_theta_max         73.38
_reflns_number_total             5611
_reflns_number_gt                4517
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0863P)²+10.9382P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5611
_refine_ls_number_parameters     394
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.1712
_refine_ls_wR_factor_gt          0.1664
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6187(3) 0.1296(11) 0.7233(5) 0.0407(17) Uani 1 1 d . . .
H1 H 0.6258 0.2067 0.7682 0.049 Uiso 1 1 calc R . .
C2 C 0.6634(3) 0.0973(12) 0.6842(5) 0.048(2) Uani 1 1 d . . .
H2 H 0.6999 0.1506 0.7037 0.057 Uiso 1 1 calc R . .
C3 C 0.6534(3) -0.0126(12) 0.6174(5) 0.0465(19) Uani 1 1 d . . .
H3 H 0.6831 -0.0354 0.5913 0.056 Uiso 1 1 calc R . .
C4 C 0.5984(3) -0.0907(10) 0.5881(4) 0.0373(16) Uani 1 1 d . . .
C5 C 0.5825(4) -0.2031(11) 0.5165(4) 0.046(2) Uani 1 1 d . . .
H5 H 0.6103 -0.2308 0.4878 0.055 Uiso 1 1 calc R . .
C6 C 0.5277(4) -0.2690(11) 0.4904(4) 0.047(2) Uani 1 1 d . . .
H6 H 0.5181 -0.3368 0.4426 0.057 Uiso 1 1 calc R . .
C7 C 0.4840(4) -0.2379(10) 0.5339(4) 0.0409(18) Uani 1 1 d . . .
C8 C 0.4259(4) -0.3031(11) 0.5107(5) 0.046(2) Uani 1 1 d . . .
H8 H 0.4139 -0.3739 0.4642 0.056 Uiso 1 1 calc R . .
C9 C 0.3878(4) -0.2622(11) 0.5566(5) 0.048(2) Uani 1 1 d . . .
H9 H 0.3496 -0.3051 0.5417 0.057 Uiso 1 1 calc R . .
C10 C 0.4063(3) -0.1555(10) 0.6259(4) 0.0385(16) Uani 1 1 d . . .
H10 H 0.3797 -0.1288 0.6567 0.046 Uiso 1 1 calc R . .
C11 C 0.4987(3) -0.1309(9) 0.6054(4) 0.0310(14) Uani 1 1 d . . .
C12 C 0.5560(3) -0.0555(10) 0.6315(4) 0.0313(14) Uani 1 1 d . . .
C13 C 0.1274(3) 0.9428(10) 0.7687(5) 0.0372(16) Uani 1 1 d . . .
H13 H 0.1278 0.8875 0.8183 0.045 Uiso 1 1 calc R . .
C14 C 0.1795(3) 0.9549(11) 0.7441(5) 0.0434(18) Uani 1 1 d . . .
H14 H 0.2142 0.9121 0.7778 0.052 Uiso 1 1 calc R . .
C15 C 0.1793(3) 1.0310(11) 0.6694(5) 0.0454(19) Uani 1 1 d . . .
H15 H 0.2136 1.0381 0.6518 0.054 Uiso 1 1 calc R . .
C16 C 0.1267(3) 1.0971(11) 0.6206(4) 0.0367(15) Uani 1 1 d . . .
C17 C 0.1213(4) 1.1767(12) 0.5415(5) 0.0447(18) Uani 1 1 d . . .
H17 H 0.1541 1.1851 0.5206 0.054 Uiso 1 1 calc R . .
C18 C 0.0695(4) 1.2394(10) 0.4970(4) 0.0400(17) Uani 1 1 d . . .
H18 H 0.0673 1.2898 0.4460 0.048 Uiso 1 1 calc R . .
C19 C 0.0178(3) 1.2296(10) 0.5272(4) 0.0341(15) Uani 1 1 d . . .
C20 C -0.0372(4) 1.2923(11) 0.4844(4) 0.0403(17) Uani 1 1 d . . .
H20 H -0.0425 1.3390 0.4321 0.048 Uiso 1 1 calc R . .
C21 C -0.0831(3) 1.2840(11) 0.5205(4) 0.0417(17) Uani 1 1 d . . .
H21 H -0.1194 1.3301 0.4938 0.050 Uiso 1 1 calc R . .
C22 C -0.0751(3) 1.2054(11) 0.5982(4) 0.0354(15) Uani 1 1 d . . .
H22 H -0.1067 1.2003 0.6218 0.043 Uiso 1 1 calc R . .
C23 C 0.0220(3) 1.1517(9) 0.6046(4) 0.0304(14) Uani 1 1 d . . .
C24 C 0.0767(3) 1.0836(10) 0.6512(4) 0.0316(14) Uani 1 1 d . . .
C25 C 0.7576(4) 0.5342(10) 0.6808(4) 0.0424(18) Uani 1 1 d . B .
C26 C 0.7035(5) 0.5616(12) 0.6954(7) 0.068(3) Uani 1 1 d D . .
H26 H 0.6700 0.5786 0.6540 0.082 Uiso 1 1 calc R A 1
C27 C 0.7030(12) 0.562(2) 0.7778(11) 0.133(12) Uani 0.84(3) 1 d PD B 1
H27 H 0.6675 0.5802 0.7912 0.160 Uiso 0.84(3) 1 calc PR B 1
C28 C 0.7513(13) 0.537(3) 0.8391(12) 0.22(3) Uani 0.84(3) 1 d PD B 1
H28 H 0.7477 0.5369 0.8925 0.263 Uiso 0.84(3) 1 calc PR B 1
C29 C 0.8048(13) 0.511(2) 0.8244(7) 0.172(16) Uani 0.84(3) 1 d PD B 1
H29 H 0.8385 0.4988 0.8660 0.206 Uiso 0.84(3) 1 calc PR B 1
C28' C 0.7259(11) 0.532(8) 0.824(2) 0.030(14) Uiso 0.16(3) 1 d PD B 2
H28' H 0.7217 0.5375 0.8774 0.036 Uiso 0.16(3) 1 calc PR B 2
C27' C 0.6780(12) 0.561(11) 0.7604(16) 0.033(14) Uiso 0.16(3) 1 d PD B 2
H27' H 0.6390 0.5756 0.7609 0.040 Uiso 0.16(3) 1 calc PR B 2
C29' C 0.7797(12) 0.495(7) 0.8107(17) 0.028(13) Uiso 0.16(3) 1 d PD B 2
H29' H 0.8060 0.4544 0.8575 0.033 Uiso 0.16(3) 1 calc PR B 2
C30 C 0.8054(6) 0.5035(14) 0.7438(5) 0.086(4) Uani 1 1 d D . .
H30 H 0.8405 0.4760 0.7310 0.103 Uiso 1 1 calc R B 1
N1 N 0.5665(2) 0.0539(8) 0.6984(3) 0.0316(12) Uani 1 1 d . . .
N2 N 0.4603(2) -0.0897(8) 0.6502(3) 0.0308(12) Uani 1 1 d . . .
N3 N 0.0772(2) 1.0070(9) 0.7243(3) 0.0330(12) Uani 1 1 d . . .
N4 N -0.0244(2) 1.1384(8) 0.6390(3) 0.0297(12) Uani 1 1 d . . .
O1 O 0.7099(3) 0.5566(9) 0.5273(3) 0.0616(17) Uani 1 1 d . B .
O2 O 0.8019(3) 0.3992(12) 0.5696(5) 0.081(2) Uani 1 1 d . B .
O3 O 0.7978(3) 0.7246(11) 0.5818(4) 0.073(2) Uani 1 1 d . B .
O4 O 0.6948(4) 0.8432(13) 0.4034(5) 0.086(2) Uani 1 1 d . . .
O5 O 0.7596(4) 1.0681(14) 0.5145(7) 0.110(3) Uani 1 1 d . . .
S1 S 0.76678(8) 0.5529(3) 0.58086(10) 0.0401(4) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.0739(2) 0.7500 0.0297(3) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.9969(2) 0.7500 0.0311(3) Uani 1 2 d S . .
I1 I 0.5000 0.43394(9) 0.7500 0.03722(19) Uani 1 2 d S . .
I2 I 0.0000 0.62934(9) 0.7500 0.03564(19) Uani 1 2 d S . .
H51 H 0.7393 1.0403 0.4663 0.100 Uiso 1 1 d . . .
H52 H 0.7804 0.9516 0.5535 0.100 Uiso 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.325(9) . ?
C1 C2 1.398(11) . ?
C2 C3 1.364(13) . ?
C3 C4 1.396(12) . ?
C4 C12 1.405(9) . ?
C4 C5 1.440(11) . ?
C5 C6 1.352(13) . ?
C6 C7 1.426(12) . ?
C7 C11 1.414(10) . ?
C7 C8 1.414(12) . ?
C8 C9 1.360(13) . ?
C9 C10 1.391(11) . ?
C10 N2 1.332(9) . ?
C11 N2 1.351(9) . ?
C11 C12 1.430(10) . ?
C12 N1 1.362(9) . ?
C13 N3 1.327(9) . ?
C13 C14 1.398(10) . ?
C14 C15 1.383(11) . ?
C15 C16 1.400(11) . ?
C16 C24 1.405(10) . ?
C16 C17 1.440(11) . ?
C17 C18 1.352(12) . ?
C18 C19 1.439(11) . ?
C19 C20 1.402(11) . ?
C19 C23 1.412(9) . ?
C20 C21 1.371(11) . ?
C21 C22 1.408(10) . ?
C22 N4 1.324(9) . ?
C23 N4 1.365(8) . ?
C23 C24 1.431(9) . ?
C24 N3 1.357(9) . ?
C25 C30 1.369(12) . ?
C25 C26 1.375(13) . ?
C25 S1 1.766(7) . ?
C26 C27' 1.38(2) . ?
C26 C27 1.399(15) . ?
C27 C28 1.356(17) . ?
C28 C29 1.361(18) . ?
C29 C30 1.371(15) . ?
C28' C29' 1.376(19) . ?
C28' C27' 1.379(19) . ?
C29' C30 1.412(19) . ?
N1 Cu1 1.980(5) . ?
N2 Cu1 2.099(6) . ?
N3 Cu2 1.977(5) . ?
N4 Cu2 2.102(5) . ?
O1 S1 1.426(6) . ?
O2 S1 1.440(7) . ?
O3 S1 1.455(7) . ?
Cu1 N1 1.980(5) 2_656 ?
Cu1 N2 2.099(6) 2_656 ?
Cu1 I1 2.6404(16) . ?
Cu2 N3 1.977(5) 2_556 ?
Cu2 N4 2.102(5) 2_556 ?
Cu2 I2 2.6955(17) . ?

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
N1 C1 C2 122.1(8) . . ?
C3 C2 C1 119.7(8) . . ?
C2 C3 C4 119.7(7) . . ?
C3 C4 C12 117.4(7) . . ?
C3 C4 C5 124.3(7) . . ?
C12 C4 C5 118.3(7) . . ?
C6 C5 C4 120.9(7) . . ?
C5 C6 C7 122.0(7) . . ?
C11 C7 C8 116.4(7) . . ?
C11 C7 C6 118.3(8) . . ?
C8 C7 C6 125.3(7) . . ?
C9 C8 C7 120.0(7) . . ?
C8 C9 C10 119.4(8) . . ?
N2 C10 C9 123.0(8) . . ?
N2 C11 C7 123.2(7) . . ?
N2 C11 C12 117.0(6) . . ?
C7 C11 C12 119.8(7) . . ?
N1 C12 C4 122.5(7) . . ?
N1 C12 C11 116.9(6) . . ?
C4 C12 C11 120.6(6) . . ?
N3 C13 C14 122.6(7) . . ?
C15 C14 C13 119.5(7) . . ?
C14 C15 C16 119.0(7) . . ?
C15 C16 C24 117.6(6) . . ?
C15 C16 C17 123.7(7) . . ?
C24 C16 C17 118.7(7) . . ?
C18 C17 C16 121.4(7) . . ?
C17 C18 C19 121.1(7) . . ?
C20 C19 C23 117.4(7) . . ?
C20 C19 C18 124.1(6) . . ?
C23 C19 C18 118.5(7) . . ?
C21 C20 C19 119.3(6) . . ?
C20 C21 C22 119.7(7) . . ?
N4 C22 C21 122.7(7) . . ?
N4 C23 C19 123.0(6) . . ?
N4 C23 C24 116.8(6) . . ?
C19 C23 C24 120.3(6) . . ?
N3 C24 C16 123.1(6) . . ?
N3 C24 C23 117.0(6) . . ?
C16 C24 C23 120.0(6) . . ?
C30 C25 C26 120.6(9) . . ?
C30 C25 S1 119.3(8) . . ?
C26 C25 S1 119.9(7) . . ?
C25 C26 C27' 138.6(17) . . ?
C25 C26 C27 114.5(15) . . ?
C27' C26 C27 24.6(14) . . ?
C28 C27 C26 123.6(17) . . ?
C27 C28 C29 121.7(17) . . ?
C28 C29 C30 115.1(17) . . ?
C29' C28' C27' 121(3) . . ?
C26 C27' C28' 101(2) . . ?
C28' C29' C30 136(3) . . ?
C25 C30 C29 124.3(16) . . ?
C25 C30 C29' 101.5(17) . . ?
C29 C30 C29' 24.5(14) . . ?
C1 N1 C12 118.5(6) . . ?
C1 N1 Cu1 127.3(5) . . ?
C12 N1 Cu1 114.1(4) . . ?
C10 N2 C11 118.0(6) . . ?
C10 N2 Cu1 131.4(5) . . ?
C11 N2 Cu1 110.6(4) . . ?
C13 N3 C24 118.2(6) . . ?
C13 N3 Cu2 127.3(5) . . ?
C24 N3 Cu2 114.5(4) . . ?
C22 N4 C23 117.9(6) . . ?
C22 N4 Cu2 131.8(5) . . ?
C23 N4 Cu2 110.2(4) . . ?
O1 S1 O2 114.5(4) . . ?
O1 S1 O3 112.6(4) . . ?
O2 S1 O3 111.9(5) . . ?
O1 S1 C25 107.1(4) . . ?
O2 S1 C25 106.0(4) . . ?
O3 S1 C25 103.6(4) . . ?
N1 Cu1 N1 171.5(4) 2_656 . ?
N1 Cu1 N2 93.8(2) 2_656 . ?
N1 Cu1 N2 81.3(2) . . ?
N1 Cu1 N2 81.3(2) 2_656 2_656 ?
N1 Cu1 N2 93.8(2) . 2_656 ?
N2 Cu1 N2 110.3(3) . 2_656 ?
N1 Cu1 I1 94.24(18) 2_656 . ?
N1 Cu1 I1 94.24(18) . . ?
N2 Cu1 I1 124.86(16) . . ?
N2 Cu1 I1 124.86(16) 2_656 . ?
N3 Cu2 N3 175.7(4) 2_556 . ?
N3 Cu2 N4 81.4(2) 2_556 2_556 ?
N3 Cu2 N4 96.5(2) . 2_556 ?
N3 Cu2 N4 96.5(2) 2_556 . ?
N3 Cu2 N4 81.4(2) . . ?
N4 Cu2 N4 120.8(3) 2_556 . ?
N3 Cu2 I2 92.15(19) 2_556 . ?
N3 Cu2 I2 92.15(19) . . ?
N4 Cu2 I2 119.59(15) 2_556 . ?
N4 Cu2 I2 119.59(15) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        73.38
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.149


