#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/96/2209650.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2209650
loop_
_publ_author_name
'Tian-Tian Pan'
'Jia-Geng Liu'
'Duan-Jun Xu'
_publ_section_title
;Bis(4-hydroxybenzoato-κO)bis(1,10-phenanthroline-κ²N,N')cadmium(II)
 dihydrate
;
_journal_coeditor_code           SG2036
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1597
_journal_page_last               m1599
_journal_paper_doi               10.1107/S1600536806021787
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Cd (C7 H5 O3)2 (C12 H8 N2)2], 2H2 O'
_chemical_formula_moiety         'C38 H26 Cd N4 O6, 2H2 O'
_chemical_formula_sum            'C38 H30 Cd N4 O8'
_chemical_formula_weight         783.06
_chemical_name_systematic
;
Bis(4-hydroxybenzoato-\kO)bis(1,10-phenanthroline-κ²N,N')cadmium(II)
dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 99.416(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.158(11)
_cell_length_b                   9.399(3)
_cell_length_c                   16.802(5)
_cell_measurement_reflns_used    15642
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.3
_cell_volume                     3608(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.025
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17121
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.033
_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)+(0.0723P)²+1.9122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.105
_refine_ls_wR_factor_ref         0.108
_reflns_number_gt                3771
_reflns_number_total             4123
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sg2036.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2209650
_cod_database_fobs_code          2209650
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.5000 0.64458(3) 0.2500 0.03886(11) Uani d S 1 . .
C C1 0.40389(13) 0.9116(3) 0.2379(2) 0.0568(7) Uani d . 1 . .
H H1 0.4035 0.9017 0.1828 0.068 Uiso calc R 1 . .
C C2 0.36625(15) 1.0092(4) 0.2641(3) 0.0740(10) Uani d . 1 . .
H H2 0.3415 1.0636 0.2269 0.089 Uiso calc R 1 . .
C C3 0.36560(15) 1.0253(4) 0.3439(3) 0.0736(10) Uani d . 1 . .
H H4 0.3401 1.0899 0.3617 0.088 Uiso calc R 1 . .
C C4 0.40350(13) 0.9443(3) 0.3996(2) 0.0579(7) Uani d . 1 . .
C C5 0.40675(18) 0.9543(4) 0.4854(2) 0.0755(10) Uani d . 1 . .
H H5 0.3814 1.0157 0.5061 0.091 Uiso calc R 1 . .
C C6 0.4449(2) 0.8784(4) 0.5364(2) 0.0716(10) Uani d . 1 . .
H H6 0.4458 0.8876 0.5917 0.086 Uiso calc R 1 . .
C C7 0.48468(15) 0.7828(3) 0.50669(17) 0.0570(7) Uani d . 1 . .
C C8 0.52670(19) 0.7027(4) 0.55738(18) 0.0738(10) Uani d . 1 . .
H H8 0.5292 0.7095 0.6131 0.089 Uiso calc R 1 . .
C C9 0.5632(2) 0.6165(5) 0.5261(2) 0.0804(11) Uani d . 1 . .
H H9 0.5913 0.5639 0.5596 0.096 Uiso calc R 1 . .
C C10 0.55826(17) 0.6069(4) 0.44265(19) 0.0665(9) Uani d . 1 . .
H H10 0.5836 0.5465 0.4213 0.080 Uiso calc R 1 . .
C C11 0.48255(12) 0.7676(3) 0.42311(14) 0.0436(5) Uani d . 1 . .
C C12 0.44102(12) 0.8493(2) 0.36792(18) 0.0439(5) Uani d . 1 . .
C C13 0.38388(10) 0.4761(3) 0.25277(14) 0.0410(5) Uani d . 1 . .
C C14 0.33523(10) 0.3825(3) 0.21265(16) 0.0399(5) Uani d . 1 . .
C C15 0.33649(12) 0.3228(3) 0.13729(17) 0.0487(6) Uani d . 1 . .
H H15 0.3685 0.3405 0.1117 0.058 Uiso calc R 1 . .
C C16 0.29160(12) 0.2379(3) 0.09939(16) 0.0517(6) Uani d . 1 . .
H H16 0.2928 0.2021 0.0481 0.062 Uiso calc R 1 . .
C C17 0.24468(11) 0.2063(3) 0.13808(16) 0.0455(5) Uani d . 1 . .
C C18 0.24310(11) 0.2618(3) 0.21406(17) 0.0478(6) Uani d . 1 . .
H H18 0.2120 0.2398 0.2406 0.057 Uiso calc R 1 . .
C C19 0.28774(12) 0.3503(3) 0.25087(18) 0.0456(6) Uani d . 1 . .
H H19 0.2859 0.3884 0.3015 0.055 Uiso calc R 1 . .
N N1 0.44028(10) 0.8320(2) 0.28788(14) 0.0444(5) Uani d . 1 . .
N N2 0.51916(11) 0.6798(3) 0.39205(13) 0.0479(5) Uani d . 1 . .
O O1 0.43043(8) 0.4755(2) 0.22214(12) 0.0539(5) Uani d . 1 . .
O O2 0.37743(8) 0.5486(2) 0.31302(12) 0.0513(4) Uani d . 1 . .
O O3 0.20243(10) 0.1196(2) 0.09953(14) 0.0597(5) Uani d . 1 . .
H H3 0.1797 0.1032 0.1314 0.080 Uiso d R 1 . .
O O1W 0.5000 0.2117(5) 0.2500 0.0887(11) Uani d S 1 . .
H H1A 0.4662 0.2768 0.2390 0.080 Uiso d R 1 . .
O O2A 0.2680(12) 0.149(2) 0.5350(17) 0.170(9) Uiso d P 0.25 A 1
H H2A 0.2595 0.0885 0.4976 0.255 Uiso d PR 0.25 A 1
H H2B 0.2873 0.1092 0.5756 0.255 Uiso d PR 0.25 A 1
O O2B 0.2665(9) 0.277(2) 0.5266(12) 0.140(6) Uiso d P 0.25 B 2
H H2C 0.2652 0.3617 0.5538 0.210 Uiso d PR 0.25 B 2
H H2D 0.2629 0.3014 0.4758 0.210 Uiso d PR 0.25 B 2
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cd O1 . 2_655 90.47(11) y
O1 Cd N1 . . 98.61(8) y
O1 Cd N1 . 2_655 152.69(8) y
O1 Cd N2 . . 108.40(8) y
O1 Cd N2 . 2_655 83.12(8) y
N1 Cd N1 . 2_655 85.02(11) y
N1 Cd N2 . . 69.59(8) y
N1 Cd N2 . 2_655 98.27(8) y
N2 Cd N2 . 2_655 164.01(12) y
N2 Cd O1 . 2_655 83.12(8) ?
O1 Cd N1 2_655 2_655 98.61(8) ?
O1 Cd N2 2_655 2_655 108.40(8) ?
N1 Cd O1 . 2_655 152.69(8) ?
N2 Cd N1 . 2_655 98.27(8) ?
N2 Cd N1 . 2_655 98.27(8) ?
N2 Cd N1 2_655 2_655 69.59(8) ?
N2 Cd N1 . 2_655 98.27(8) ?
N1 C1 C2 . . 122.8(3) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C3 C2 C1 . . 119.9(3) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 119.7(3) ?
C2 C3 H4 . . 120.2 ?
C4 C3 H4 . . 120.2 ?
C3 C4 C12 . . 116.8(3) ?
C3 C4 C5 . . 124.1(3) ?
C12 C4 C5 . . 119.1(3) ?
C6 C5 C4 . . 122.1(3) ?
C6 C5 H5 . . 118.9 ?
C4 C5 H5 . . 118.9 ?
C5 C6 C7 . . 120.5(3) ?
C5 C6 H6 . . 119.8 ?
C7 C6 H6 . . 119.8 ?
C8 C7 C11 . . 117.4(3) ?
C8 C7 C6 . . 123.1(3) ?
C11 C7 C6 . . 119.5(3) ?
C9 C8 C7 . . 120.4(3) ?
C9 C8 H8 . . 119.8 ?
C7 C8 H8 . . 119.8 ?
C8 C9 C10 . . 118.8(3) ?
C8 C9 H9 . . 120.6 ?
C10 C9 H9 . . 120.6 ?
N2 C10 C9 . . 123.2(3) ?
N2 C10 H10 . . 118.4 ?
C9 C10 H10 . . 118.4 ?
N2 C11 C7 . . 121.9(3) ?
N2 C11 C12 . . 118.2(2) ?
C7 C11 C12 . . 119.9(3) ?
N1 C12 C4 . . 122.9(3) ?
N1 C12 C11 . . 118.3(2) ?
C4 C12 C11 . . 118.8(3) ?
O2 C13 O1 . . 123.6(2) ?
O2 C13 C14 . . 120.2(2) ?
O1 C13 C14 . . 116.1(2) ?
C15 C14 C19 . . 117.9(2) ?
C15 C14 C13 . . 121.3(2) ?
C19 C14 C13 . . 120.8(2) ?
C16 C15 C14 . . 121.8(2) ?
C16 C15 H15 . . 119.1 ?
C14 C15 H15 . . 119.1 ?
C15 C16 C17 . . 119.8(3) ?
C15 C16 H16 . . 120.1 ?
C17 C16 H16 . . 120.1 ?
O3 C17 C18 . . 122.8(2) ?
O3 C17 C16 . . 117.7(3) ?
C18 C17 C16 . . 119.5(2) ?
C17 C18 C19 . . 120.4(2) ?
C17 C18 H18 . . 119.8 ?
C19 C18 H18 . . 119.8 ?
C18 C19 C14 . . 120.7(3) ?
C18 C19 H19 . . 119.7 ?
C14 C19 H19 . . 119.7 ?
C1 N1 C12 . . 117.9(3) ?
C1 N1 Cd . . 125.8(2) ?
C12 N1 Cd . . 116.09(16) ?
C10 N2 C11 . . 118.3(2) ?
C10 N2 Cd . . 124.6(2) ?
C11 N2 Cd . . 116.60(16) ?
C13 O1 Cd . . 122.53(18) ?
C17 O3 H3 . . 106.9 ?
H2A O2A H2B . . 109.8 ?
H2C O2B H2D . . 104.8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cd O1 . 2.257(2) y
Cd N1 . 2.389(2) y
Cd N2 . 2.378(2) y
Cd O1 2_655 2.257(2) ?
Cd N1 2_655 2.389(2) ?
Cd N2 2_655 2.378(2) ?
C1 N1 . 1.320(4) ?
C1 C2 . 1.386(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.352(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.398(5) ?
C3 H4 . 0.9300 ?
C4 C12 . 1.410(4) ?
C4 C5 . 1.433(5) ?
C5 C6 . 1.334(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.434(5) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.403(5) ?
C7 C11 . 1.404(4) ?
C8 C9 . 1.338(6) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.391(5) ?
C9 H9 . 0.9300 ?
C10 N2 . 1.327(4) ?
C10 H10 . 0.9300 ?
C11 N2 . 1.348(3) ?
C11 C12 . 1.443(4) ?
C12 N1 . 1.352(4) ?
C13 O2 . 1.249(3) ?
C13 O1 . 1.268(3) ?
C13 C14 . 1.500(3) ?
C14 C15 . 1.390(4) ?
C14 C19 . 1.394(4) ?
C15 C16 . 1.380(4) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.387(4) ?
C16 H16 . 0.9300 ?
C17 O3 . 1.354(3) ?
C17 C18 . 1.385(4) ?
C18 C19 . 1.390(4) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
O3 H3 . 0.8257 ?
O1W H1A . 0.9869 ?
O2A H2A . 0.8440 ?
O2A H2B . 0.8375 ?
O2B H2C . 0.9192 ?
O2B H2D . 0.8738 ?
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 H1A O1 . 0.99 2.04 2.952(5) 152 y
O3 H3 O2 4_545 0.82 1.81 2.629(3) 170 y
