#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/16/8101699.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_8101699
loop_
_publ_author_name
'S.-R. Fan'
'L.-P. Zhang'
'H.-P. Xiao'
'G.-Q. Cai'
'L.-G. Zhu'
_publ_section_title
;
Crystal structure of bis[diaqua(1,10-phenanthroline)(μ-4-sulfobenzoato)
cadmium(II)], [Cd(H₂O)₂(C₁₂H₈N₂)(C₇H₄O₅S)]₂
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              69
_journal_page_last               70
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         'C38 H32 Cd2 N4 O14 S2'
_chemical_formula_sum            'C38 H32 Cd2 N4 O14 S2'
_chemical_formula_weight         1057.60
_chemical_name_systematic
;
 bis[diaqua(1,10-phenanthroline)(μ-4-sulfobenzoato)cadmium(II)]
;
_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                102.000(2)
_cell_angle_beta                 101.049(2)
_cell_angle_gamma                113.4530(10)
_cell_formula_units_Z            1
_cell_length_a                   8.2384(8)
_cell_length_b                   10.1299(9)
_cell_length_c                   12.9685(12)
_cell_measurement_reflns_used    8023
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.4
_cell_measurement_theta_min      3.4
_cell_volume                     924.65(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6782
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  0.9002
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0518
_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)+(0.0211P)²+3.3727P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                3208
_reflns_number_total             3274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1429.cff
_cod_data_source_block           x59-lgzhu
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101699
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_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.75349(6) 0.65201(4) 0.21276(3) 0.03123(14) Uani 1 2 i d . . .
S1 S 0.7912(2) 1.25926(16) -0.18994(12) 0.0347(3) Uani 1 2 i d . . .
O1 O 0.6528(6) 0.7159(5) 0.0561(4) 0.0466(11) Uani 1 2 i d . . .
O2 O 0.8334(6) 0.9152(5) 0.2016(3) 0.0501(11) Uani 1 2 i d . . .
O3 O 0.9279(6) 1.2497(5) -0.2426(3) 0.0441(10) Uani 1 2 i d . . .
O4 O 0.6105(7) 1.1973(6) -0.2678(5) 0.0757(17) Uani 1 2 i d . . .
O5 O 0.8554(7) 1.4128(5) -0.1185(4) 0.0569(13) Uani 1 2 i d . . .
O6 O 0.4268(6) 0.4814(5) 0.1612(4) 0.0405(10) Uani 1 2 i d D . .
O7 O 0.7259(6) 0.4484(5) 0.0724(4) 0.0422(10) Uani 1 2 i d D . .
N1 N 0.7601(6) 0.7553(5) 0.3910(4) 0.0322(10) Uani 1 2 i d . . .
N2 N 0.7840(6) 0.4925(5) 0.3210(4) 0.0326(10) Uani 1 2 i d . . .
C1 C 0.7558(9) 0.8860(7) 0.4274(5) 0.0433(15) Uani 1 2 i d . . .
H1 H 0.7562 0.9430 0.3797 0.052 Uiso 1 2 i calc R . .
C2 C 0.7508(10) 0.9413(8) 0.5328(5) 0.0530(17) Uani 1 2 i d . . .
H2 H 0.7530 1.0354 0.5558 0.064 Uiso 1 2 i calc R . .
C3 C 0.7426(9) 0.8580(8) 0.6023(5) 0.0523(17) Uani 1 2 i d . . .
H3 H 0.7378 0.8940 0.6732 0.063 Uiso 1 2 i calc R . .
C4 C 0.7415(8) 0.7178(7) 0.5673(5) 0.0410(15) Uani 1 2 i d . . .
C5 C 0.7246(9) 0.6200(9) 0.6333(5) 0.0521(18) Uani 1 2 i d . . .
H5 H 0.7104 0.6484 0.7027 0.063 Uiso 1 2 i calc R . .
C6 C 0.7289(9) 0.4868(9) 0.5972(6) 0.057(2) Uani 1 2 i d . . .
H6 H 0.7162 0.4246 0.6418 0.068 Uiso 1 2 i calc R . .
C7 C 0.7526(8) 0.4398(7) 0.4920(5) 0.0439(15) Uani 1 2 i d . . .
C8 C 0.7680(9) 0.3069(8) 0.4526(6) 0.0546(19) Uani 1 2 i d . . .
H8 H 0.7604 0.2429 0.4955 0.066 Uiso 1 2 i calc R . .
C9 C 0.7938(9) 0.2714(7) 0.3529(6) 0.0514(17) Uani 1 2 i d . . .
H9 H 0.8069 0.1845 0.3274 0.062 Uiso 1 2 i calc R . .
C10 C 0.8006(8) 0.3670(7) 0.2887(5) 0.0428(15) Uani 1 2 i d . . .
H10 H 0.8176 0.3413 0.2199 0.051 Uiso 1 2 i calc R . .
C11 C 0.7541(7) 0.6712(6) 0.4596(4) 0.0326(12) Uani 1 2 i d . . .
C12 C 0.7628(7) 0.5303(6) 0.4218(4) 0.0317(12) Uani 1 2 i d . . .
C13 C 0.7466(8) 0.8594(7) 0.1019(5) 0.0355(13) Uani 1 2 i d . . .
C14 C 0.7534(8) 0.9596(6) 0.0305(4) 0.0313(12) Uani 1 2 i d . . .
C15 C 0.6231(8) 0.9069(7) -0.0719(5) 0.0420(15) Uani 1 2 i d . . .
H15 H 0.5278 0.8081 -0.0969 0.050 Uiso 1 2 i calc R . .
C16 C 0.6327(8) 0.9994(6) -0.1378(5) 0.0396(14) Uani 1 2 i d . . .
H16 H 0.5430 0.9636 -0.2061 0.047 Uiso 1 2 i calc R . .
C17 C 0.7754(7) 1.1444(6) -0.1018(4) 0.0296(12) Uani 1 2 i d . . .
C18 C 0.9062(8) 1.1988(6) 0.0009(5) 0.0369(13) Uani 1 2 i d . . .
H18 H 1.0022 1.2972 0.0254 0.044 Uiso 1 2 i calc R . .
C19 C 0.8941(8) 1.1071(6) 0.0665(5) 0.0361(13) Uani 1 2 i d . . .
H19 H 0.9813 1.1445 0.1359 0.043 Uiso 1 2 i calc R . .
H7A H 0.624(4) 0.396(6) 0.026(4) 0.050 Uiso 1 2 i d D . .
H6B H 0.400(9) 0.420(6) 0.101(3) 0.050 Uiso 1 2 i d D . .
H6A H 0.372(8) 0.533(6) 0.157(6) 0.050 Uiso 1 2 i d D . .
H7B H 0.821(5) 0.466(7) 0.055(5) 0.050 Uiso 1 2 i d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cd Cd -0.8075 1.2024 '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 Cd1 O3 98.20(15) . 2_775 ?
N1 Cd1 O7 150.58(16) . . ?
O3 Cd1 O7 86.16(14) 2_775 . ?
N1 Cd1 O1 126.10(15) . . ?
O3 Cd1 O1 102.79(15) 2_775 . ?
O7 Cd1 O1 80.39(15) . . ?
N1 Cd1 N2 70.63(15) . . ?
O3 Cd1 N2 86.96(15) 2_775 . ?
O7 Cd1 N2 80.64(16) . . ?
O1 Cd1 N2 157.99(15) . . ?
N1 Cd1 O6 91.71(15) . . ?
O3 Cd1 O6 163.13(14) 2_775 . ?
O7 Cd1 O6 78.60(14) . . ?
O1 Cd1 O6 81.92(14) . . ?
N2 Cd1 O6 83.48(15) . . ?
N1 Cd1 O2 83.89(15) . . ?
O3 Cd1 O2 78.98(15) 2_775 . ?
O7 Cd1 O2 125.37(15) . . ?
O1 Cd1 O2 53.20(14) . . ?
N2 Cd1 O2 148.81(15) . . ?
O6 Cd1 O2 115.82(14) . . ?
O4 S1 O3 112.4(3) . . ?
O4 S1 O5 113.5(3) . . ?
O3 S1 O5 111.0(3) . . ?
O4 S1 C17 107.0(3) . . ?
O3 S1 C17 105.9(2) . . ?
O5 S1 C17 106.4(3) . . ?
C13 O1 Cd1 95.8(3) . . ?
C13 O2 Cd1 89.2(3) . . ?
S1 O3 Cd1 142.2(3) . 2_775 ?
Cd1 O6 H6B 107(5) . . ?
Cd1 O6 H6A 107(5) . . ?
H6B O6 H6A 112(7) . . ?
Cd1 O7 H7A 116(5) . . ?
Cd1 O7 H7B 113(5) . . ?
H7A O7 H7B 121(7) . . ?
C1 N1 C11 118.1(5) . . ?
C1 N1 Cd1 124.4(4) . . ?
C11 N1 Cd1 117.3(4) . . ?
C10 N2 C12 118.0(5) . . ?
C10 N2 Cd1 127.4(4) . . ?
C12 N2 Cd1 114.3(3) . . ?
N1 C1 C2 123.1(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.6(6) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C11 117.4(5) . . ?
C3 C4 C5 123.2(6) . . ?
C11 C4 C5 119.3(6) . . ?
C6 C5 C4 121.2(6) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 121.2(6) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C12 116.7(6) . . ?
C8 C7 C6 123.8(6) . . ?
C12 C7 C6 119.6(6) . . ?
C9 C8 C7 120.4(6) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 123.2(6) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N1 C11 C4 122.0(5) . . ?
N1 C11 C12 118.6(5) . . ?
C4 C11 C12 119.4(5) . . ?
N2 C12 C7 122.8(5) . . ?
N2 C12 C11 118.1(5) . . ?
C7 C12 C11 119.1(5) . . ?
O2 C13 O1 121.4(5) . . ?
O2 C13 C14 120.3(5) . . ?
O1 C13 C14 118.3(5) . . ?
C15 C14 C19 118.8(5) . . ?
C15 C14 C13 121.2(5) . . ?
C19 C14 C13 119.9(5) . . ?
C14 C15 C16 120.7(5) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 119.7(5) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.1(5) . . ?
C16 C17 S1 119.2(4) . . ?
C18 C17 S1 120.7(4) . . ?
C19 C18 C17 119.8(5) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C14 120.8(5) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
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
Cd1 N1 2.311(4) . ?
Cd1 O3 2.324(4) 2_775 ?
Cd1 O7 2.350(4) . ?
Cd1 O1 2.359(4) . ?
Cd1 N2 2.403(4) . ?
Cd1 O6 2.409(5) . ?
Cd1 O2 2.522(4) . ?
S1 O4 1.431(5) . ?
S1 O3 1.448(4) . ?
S1 O5 1.454(5) . ?
S1 C17 1.780(5) . ?
O1 C13 1.278(7) . ?
O2 C13 1.234(7) . ?
O3 Cd1 2.324(4) 2_775 ?
O6 H6B 0.82(4) . ?
O6 H6A 0.82(7) . ?
O7 H7A 0.82(5) . ?
O7 H7B 0.82(5) . ?
N1 C1 1.326(7) . ?
N1 C11 1.349(7) . ?
N2 C10 1.323(7) . ?
N2 C12 1.348(7) . ?
C1 C2 1.380(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.351(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(9) . ?
C3 H3 0.9300 . ?
C4 C11 1.416(8) . ?
C4 C5 1.422(9) . ?
C5 C6 1.350(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.426(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.401(10) . ?
C7 C12 1.411(7) . ?
C8 C9 1.349(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(9) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.444(8) . ?
C13 C14 1.503(7) . ?
C14 C15 1.379(8) . ?
C14 C19 1.385(8) . ?
C15 C16 1.383(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.374(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.382(8) . ?
C18 C19 1.372(8) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O1 0.82(5) 2.03(5) 2.829(6) 165(7) 2_665
O6 H6A O5 0.82(7) 2.15(7) 2.933(6) 159(6) 2_675
O6 H6A S1 0.82(7) 2.92(7) 3.725(4) 169(6) 2_675
O6 H6B O1 0.82(4) 2.06(4) 2.876(6) 174(7) 2_665
O7 H7B O5 0.82(5) 2.30(5) 2.889(6) 129(6) 1_545
O7 H7B O5 0.82(5) 2.33(4) 3.038(7) 145(6) 2_775
