#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:26:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180339 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/08/7200805.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_7200805
loop_
_publ_author_name
'Latham, Kay'
'Mensforth, Emily J.'
'Rix, Colin J.'
'White, Jonathan M.'
_publ_section_title
;
 Synthesis of supramolecular metallo-amine-oxy acid systems via crystal
 disassembly/reassembly
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1343
_journal_paper_doi               10.1039/b822193f
_journal_volume                  11
_journal_year                    2009
_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
_chemical_melting_point          'decomposes greater than 373K'
_chemical_name_common
;
iodobis(1,10-phenanthroline)copper(ii) phenylsulphonate dihydrate
;
_chemical_name_systematic
;
iodobis(1,10-phenanthroline)copper(II) phenylsulphonate dihydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.1310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.6321(3)
_cell_length_b                   7.33380(10)
_cell_length_c                   16.9532(2)
_cell_measurement_reflns_used    7122
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.1574
_cell_measurement_theta_min      2.6877
_cell_volume                     2849.30(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14131
_diffrn_reflns_theta_full        73.38
_diffrn_reflns_theta_max         73.38
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    10.678
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.060
_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_crystal_colour            black
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.5681
_exptl_crystal_size_mid          0.3403
_exptl_crystal_size_min          0.0300
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5611
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0863P)²+10.9382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                4517
_reflns_number_total             5611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822193f.txt
_cod_data_source_block           jmwks6a
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7200805
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_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 . . .
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'
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) . . ?
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) . ?
