#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/73/2217368.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_2217368
loop_
_publ_author_name
'Chao Qin'
_publ_section_title
Bis(3,5-dicarboxybenzoato-κ²O,O')(1,10-phenanthroline-κ²N,N')cadmium(II)
_journal_coeditor_code           XU2344
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m34
_journal_page_last               m34
_journal_paper_doi               10.1107/S1600536807053664
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cd (C9 H5 O6)2 (C12 H8 N2)]'
_chemical_formula_moiety         'C30 H18 Cd N2 O12'
_chemical_formula_sum            'C30 H18 Cd N2 O12'
_chemical_formula_weight         710.86
_chemical_name_systematic
Bis(3,5-dicarboxybenzoato-κ²O,O')(1,10-phenanthroline-κ²N,N')cadmium(II)
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.838(2)
_cell_length_b                   16.541(3)
_cell_length_c                   16.681(3)
_cell_measurement_reflns_used    5790
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.42
_cell_volume                     2698.0(9)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5790
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.42
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.8158
_exptl_absorpt_correction_T_min  0.7650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0296
_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)+(0.0396P)²+1.679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                2834
_reflns_number_total             3095
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2344.cif
_cod_data_source_block           I
_cod_original_cell_volume        2698.1(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2217368
_cod_database_fobs_code          2217368
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
Cd Cd1 0.0000 0.095232(10) 0.2500 0.03259(8) Uani d S 1
O O1 -0.04641(13) 0.16023(9) 0.36635(9) 0.0375(3) Uani d . 1
O O2 0.15070(14) 0.18897(9) 0.32348(10) 0.0413(3) Uani d . 1
O O3 -0.22565(16) 0.33500(11) 0.56195(12) 0.0573(5) Uani d . 1
H H3A -0.2837 0.3482 0.5911 0.086 Uiso calc R 1
O O4 -0.10746(19) 0.43487(13) 0.62596(12) 0.0609(5) Uani d . 1
O O5 0.42788(16) 0.41835(12) 0.44051(11) 0.0528(5) Uani d . 1
H H5A 0.4928 0.4496 0.4480 0.079 Uiso calc R 1
O O6 0.34627(16) 0.49693(11) 0.53307(11) 0.0512(4) Uani d . 1
N N1 0.13969(15) -0.01388(10) 0.26674(9) 0.0307(3) Uani d . 1
C C1 0.07969(18) 0.27267(11) 0.42660(11) 0.0292(3) Uani d . 1
C C2 -0.02139(18) 0.29186(12) 0.47520(12) 0.0327(4) Uani d . 1
H H2 -0.0985 0.2593 0.4745 0.039 Uiso calc R 1
C C4 -0.00817(18) 0.35978(12) 0.52518(12) 0.0328(4) Uani d . 1
C C5 0.1072(2) 0.40796(12) 0.52686(13) 0.0340(4) Uani d . 1
H H5 0.1162 0.4534 0.5599 0.041 Uiso calc R 1
C C6 0.20969(19) 0.38836(12) 0.47902(12) 0.0319(4) Uani d . 1
C C7 0.19579(18) 0.32127(12) 0.42853(12) 0.0312(4) Uani d . 1
H H7 0.2639 0.3088 0.3961 0.037 Uiso calc R 1
C C8 0.06177(17) 0.20275(11) 0.36910(11) 0.0296(3) Uani d . 1
C C9 -0.1171(2) 0.38168(14) 0.57696(14) 0.0395(4) Uani d . 1
C C10 0.2741(2) -0.01298(14) 0.28658(13) 0.0409(4) Uani d . 1
H H10 0.3193 0.0365 0.2907 0.049 Uiso calc R 1
C C11 0.3497(2) -0.08376(17) 0.30141(16) 0.0496(6) Uani d . 1
H H11 0.4434 -0.0812 0.3169 0.060 Uiso calc R 1
C C12 0.2851(2) -0.15675(15) 0.29300(15) 0.0496(6) Uani d . 1
H H12 0.3348 -0.2043 0.3020 0.060 Uiso calc R 1
C C13 0.1425(2) -0.15987(12) 0.27059(13) 0.0383(4) Uani d . 1
C C14 0.07359(18) -0.08582(10) 0.25986(11) 0.0278(3) Uani d . 1
C C15 0.0681(3) -0.23439(13) 0.26011(16) 0.0517(6) Uani d . 1
H H15 0.1146 -0.2833 0.2674 0.062 Uiso calc R 1
C C17 0.33550(19) 0.43895(13) 0.48512(12) 0.0346(4) Uani d . 1
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
N1 Cd1 N1 2 . 74.48(8)
N1 Cd1 O1 2 . 107.52(5)
N1 Cd1 O1 . . 116.15(6)
N1 Cd1 O1 2 2 116.15(6)
N1 Cd1 O1 . 2 107.52(5)
O1 Cd1 O1 . 2 124.47(8)
N1 Cd1 O2 2 . 156.02(6)
N1 Cd1 O2 . . 96.89(6)
O1 Cd1 O2 . . 55.61(5)
O1 Cd1 O2 2 . 87.71(6)
N1 Cd1 O2 2 2 96.89(6)
N1 Cd1 O2 . 2 156.02(6)
O1 Cd1 O2 . 2 87.71(6)
O1 Cd1 O2 2 2 55.61(5)
O2 Cd1 O2 . 2 99.04(8)
N1 Cd1 C8 2 . 134.67(6)
N1 Cd1 C8 . . 110.57(6)
O1 Cd1 C8 . . 28.25(5)
O1 Cd1 C8 2 . 105.31(6)
O2 Cd1 C8 . . 27.55(5)
O2 Cd1 C8 2 . 91.54(6)
N1 Cd1 C8 2 2 110.57(6)
N1 Cd1 C8 . 2 134.67(6)
O1 Cd1 C8 . 2 105.31(6)
O1 Cd1 C8 2 2 28.25(5)
O2 Cd1 C8 . 2 91.54(6)
O2 Cd1 C8 2 2 27.55(5)
C8 Cd1 C8 . 2 97.07(8)
C8 O1 Cd1 . . 92.62(11)
C8 O2 Cd1 . . 89.68(11)
C9 O3 H3A . . 109.5
C17 O5 H5A . . 109.5
C10 N1 C14 . . 119.13(17)
C10 N1 Cd1 . . 126.54(14)
C14 N1 Cd1 . . 114.20(11)
C2 C1 C7 . . 119.52(17)
C2 C1 C8 . . 120.57(16)
C7 C1 C8 . . 119.83(17)
C1 C2 C4 . . 120.49(16)
C1 C2 H2 . . 119.8
C4 C2 H2 . . 119.8
C5 C4 C2 . . 119.82(17)
C5 C4 C9 . . 119.20(18)
C2 C4 C9 . . 120.98(16)
C4 C5 C6 . . 119.90(18)
C4 C5 H5 . . 120.0
C6 C5 H5 . . 120.0
C7 C6 C5 . . 120.28(16)
C7 C6 C17 . . 121.04(18)
C5 C6 C17 . . 118.65(17)
C6 C7 C1 . . 119.98(17)
C6 C7 H7 . . 120.0
C1 C7 H7 . . 120.0
O2 C8 O1 . . 121.27(17)
O2 C8 C1 . . 119.47(16)
O1 C8 C1 . . 119.22(16)
O2 C8 Cd1 . . 62.77(10)
O1 C8 Cd1 . . 59.14(10)
C1 C8 Cd1 . . 169.85(13)
O4 C9 O3 . . 124.2(2)
O4 C9 C4 . . 124.38(18)
O3 C9 C4 . . 111.46(18)
N1 C10 C11 . . 122.1(2)
N1 C10 H10 . . 118.9
C11 C10 H10 . . 118.9
C12 C11 C10 . . 119.4(2)
C12 C11 H11 . . 120.3
C10 C11 H11 . . 120.3
C11 C12 C13 . . 119.8(2)
C11 C12 H12 . . 120.1
C13 C12 H12 . . 120.1
C14 C13 C12 . . 117.01(19)
C14 C13 C15 . . 120.15(19)
C12 C13 C15 . . 122.83(19)
N1 C14 C13 . . 122.39(17)
N1 C14 C14 . 2 118.52(10)
C13 C14 C14 . 2 119.08(12)
C15 C15 C13 2 . 120.75(12)
C15 C15 H15 2 . 119.6
C13 C15 H15 . . 119.6
O6 C17 O5 . . 124.15(17)
O6 C17 C6 . . 119.21(18)
O5 C17 C6 . . 116.62(18)
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
Cd1 N1 2 2.2671(16) ?
Cd1 N1 . 2.2671(16) y
Cd1 O1 . 2.3079(14) y
Cd1 O1 2 2.3079(14) ?
Cd1 O2 . 2.3883(15) y
Cd1 O2 2 2.3883(15) ?
Cd1 C8 . 2.6858(19) ?
Cd1 C8 2 2.6858(19) ?
O1 C8 . 1.272(2) ?
O2 C8 . 1.242(2) ?
O3 C9 . 1.319(2) ?
O3 H3A . 0.8200 ?
O4 C9 . 1.198(3) ?
O5 C17 . 1.283(3) ?
O5 H5A . 0.8200 ?
O6 C17 . 1.246(3) ?
N1 C10 . 1.327(2) ?
N1 C14 . 1.355(2) ?
C1 C2 . 1.387(3) ?
C1 C7 . 1.394(2) ?
C1 C8 . 1.500(2) ?
C2 C4 . 1.397(3) ?
C2 H2 . 0.9300 ?
C4 C5 . 1.385(2) ?
C4 C9 . 1.493(3) ?
C5 C6 . 1.391(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.391(3) ?
C6 C17 . 1.488(2) ?
C7 H7 . 0.9300 ?
C10 C11 . 1.395(3) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.364(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.412(3) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.402(3) ?
C13 C15 . 1.434(3) ?
C14 C14 2 1.449(4) ?
C15 C15 2 1.345(5) ?
C15 H15 . 0.9300 ?
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
O3 H3A O1 7_456 0.82 1.89 2.656(2) 155
O5 H5A O6 5_666 0.82 1.81 2.623(2) 170
C2 H2 O3 7_456 0.93 2.36 3.262(3) 164
