#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205265.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_2205265
loop_
_publ_author_name
'Qu, Yang'
'Liu, Zhao-Di'
'Zhu, Hai-Liang'
'Tan, Min-Yu'
_publ_section_title
catena-Poly[[aquadicinnamatocadmium]-μ-1,4-diazabicyclo[2.2.2]octane]
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m420
_journal_page_last               m422
_journal_paper_doi               10.1107/S1600536804034282
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cd(C9 H8 O2 )2 (C6 H12 N2 ) (H2 O)]'
_chemical_formula_moiety         'C24 H28 Cd N2 O5'
_chemical_formula_sum            'C24 H28 Cd N2 O5'
_chemical_formula_weight         536.88
_chemical_melting_point          453
_chemical_name_systematic
'Catena-poly [aqua dicinnamate cadmium-u-1,4-diazabicyclo[2.2.2]octane]'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   'difmap (O-H) and geom (C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1430(10)
_cell_length_b                   25.340(5)
_cell_length_c                   7.4830(10)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.37
_cell_volume                     1154.7(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5681
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.854
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0436
_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)+(0.0653P)²+0.4917P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                1943
_reflns_number_total             2113
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb6110.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2205265
_cod_database_fobs_code          2205265
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_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
_atom_site_type_symbol
Cd1 1.09927(6) 0.2500 0.32894(5) 0.02526(18) Uani d S 1 . . Cd
N1 1.1116(8) 0.2500 0.0066(7) 0.0294(11) Uani d S 1 . . N
N2 1.1084(8) 0.2500 -0.3416(6) 0.0288(10) Uani d S 1 . . N
O1 0.8042(5) 0.31261(12) 0.2889(5) 0.0478(9) Uani d . 1 . . O
O2 1.1378(5) 0.34325(14) 0.3390(5) 0.0477(9) Uani d . 1 . . O
O1W 1.4747(7) 0.2500 0.3731(6) 0.0410(11) Uani d S 1 . . O
H1 1.5618 0.2750 0.3547 0.049 Uiso d R 1 A . H
C1 0.5555(7) 0.47261(18) 0.2574(7) 0.0397(10) Uani d . 1 . . C
C2 0.3420(9) 0.4804(2) 0.1788(7) 0.0517(13) Uani d . 1 . . C
H2 0.2595 0.4518 0.1306 0.062 Uiso calc R 1 . . H
C3 0.2488(10) 0.5303(3) 0.1706(8) 0.0667(17) Uani d . 1 . . C
H3 0.1053 0.5353 0.1159 0.080 Uiso calc R 1 . . H
C4 0.3710(12) 0.5723(2) 0.2443(9) 0.0701(18) Uani d . 1 . . C
H4 0.3098 0.6059 0.2393 0.084 Uiso calc R 1 . . H
C5 0.5793(10) 0.5651(2) 0.3238(8) 0.0640(17) Uani d . 1 . . C
H5 0.6594 0.5937 0.3749 0.077 Uiso calc R 1 . . H
C6 0.6747(10) 0.5157(2) 0.3301(8) 0.0515(13) Uani d . 1 . . C
H6 0.8192 0.5113 0.3832 0.062 Uiso calc R 1 . . H
C7 0.6471(8) 0.41886(18) 0.2649(7) 0.0411(11) Uani d . 1 A . C
H7 0.5481 0.3914 0.2359 0.049 Uiso calc R 1 . . H
C8 0.8535(8) 0.40557(17) 0.3081(7) 0.0415(11) Uani d . 1 . . C
H8 0.9551 0.4324 0.3382 0.050 Uiso calc R 1 A . H
C9 0.9345(8) 0.35101(17) 0.3119(6) 0.0358(10) Uani d . 1 . . C
C10 0.8949(14) 0.2619(4) -0.0857(12) 0.047(3) Uiso d P 0.50 A -1 C
H10A 0.8495 0.2965 -0.0489 0.056 Uiso calc PR 0.50 A -1 H
H10B 0.7906 0.2362 -0.0522 0.056 Uiso calc PR 0.50 A -1 H
C11 0.8941(13) 0.2611(4) -0.2918(11) 0.044(3) Uiso d P 0.50 A -1 C
H11A 0.7914 0.2344 -0.3439 0.053 Uiso calc PR 0.50 A -1 H
H11B 0.8440 0.2950 -0.3412 0.053 Uiso calc PR 0.50 A -1 H
C12 1.277(2) 0.2879(5) -0.0462(18) 0.059(3) Uiso d P 0.50 A -1 C
H12A 1.4213 0.2788 0.0147 0.070 Uiso calc PR 0.50 A -1 H
H12B 1.2415 0.3233 -0.0102 0.070 Uiso calc PR 0.50 A -1 H
C13 1.278(3) 0.2859(6) -0.259(2) 0.080(5) Uiso d P 0.50 A -1 C
H13A 1.2522 0.3210 -0.3086 0.096 Uiso calc PR 0.50 A -1 H
H13B 1.4207 0.2741 -0.2847 0.096 Uiso calc PR 0.50 A -1 H
C14 1.1992(18) 0.3007(4) -0.0556(14) 0.038(2) Uiso d P 0.50 A -2 C
H14A 1.3473 0.3061 0.0044 0.046 Uiso calc PR 0.50 A -2 H
H14B 1.1090 0.3297 -0.0230 0.046 Uiso calc PR 0.50 A -2 H
C15 1.2013(17) 0.3007(4) -0.2605(14) 0.037(2) Uiso d P 0.50 A -2 C
H15A 1.1151 0.3301 -0.3138 0.044 Uiso calc PR 0.50 A -2 H
H15B 1.3508 0.3050 -0.2866 0.044 Uiso calc PR 0.50 A -2 H
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
O1W Cd1 O2 . . 84.31(8) y
O1W Cd1 O2 . 4_565 84.31(8) y
O2 Cd1 O2 . 4_565 168.45(16) y
O1W Cd1 O1 . 4_565 138.56(7) y
O2 Cd1 O1 . 4_565 137.13(11) y
O2 Cd1 O1 4_565 4_565 54.29(11) y
O1W Cd1 O1 . . 138.56(7) y
O2 Cd1 O1 . . 54.29(11) y
O2 Cd1 O1 4_565 . 137.13(11) y
O1 Cd1 O1 4_565 . 82.86(15) y
O1W Cd1 N1 . . 88.88(16) y
O2 Cd1 N1 . . 90.89(9) y
O2 Cd1 N1 4_565 . 90.89(9) y
O1 Cd1 N1 4_565 . 89.88(13) y
O1 Cd1 N1 . . 89.88(13) y
O1W Cd1 N2 . 1_556 88.05(16) y
O2 Cd1 N2 . 1_556 88.81(9) y
O2 Cd1 N2 4_565 1_556 88.81(8) y
O1 Cd1 N2 4_565 1_556 92.42(13) y
O1 Cd1 N2 . 1_556 92.42(13) y
N1 Cd1 N2 . 1_556 176.93(15) y
O1W Cd1 C9 . 4_565 111.41(10) ?
O2 Cd1 C9 . 4_565 164.22(14) ?
O2 Cd1 C9 4_565 4_565 27.10(12) ?
O1 Cd1 C9 4_565 4_565 27.19(13) ?
O1 Cd1 C9 . 4_565 110.03(13) ?
N1 Cd1 C9 . 4_565 90.78(10) ?
N2 Cd1 C9 1_556 4_565 90.34(10) ?
O1W Cd1 C9 . . 111.41(10) ?
O2 Cd1 C9 . . 27.10(12) ?
O2 Cd1 C9 4_565 . 164.22(14) ?
O1 Cd1 C9 4_565 . 110.03(12) ?
O1 Cd1 C9 . . 27.19(13) ?
N1 Cd1 C9 . . 90.78(10) ?
N2 Cd1 C9 1_556 . 90.34(10) ?
C9 Cd1 C9 4_565 . 137.2(2) ?
C10 N1 C12 4_565 . 128.7(7) ?
C10 N1 C12 . . 110.8(7) ?
C10 N1 C12 4_565 4_565 110.8(7) ?
C10 N1 C12 . 4_565 128.7(7) ?
C12 N1 C12 . 4_565 80.3(11) ?
C10 N1 C14 4_565 4_565 91.1(6) ?
C10 N1 C14 . 4_565 112.2(6) ?
C12 N1 C14 . 4_565 100.7(8) ?
C10 N1 C14 4_565 . 112.2(6) ?
C10 N1 C14 . . 91.1(6) ?
C12 N1 C14 4_565 . 100.7(8) ?
C14 N1 C14 4_565 . 119.0(9) ?
C10 N1 Cd1 4_565 . 109.1(4) ?
C10 N1 Cd1 . . 109.1(4) ?
C12 N1 Cd1 . . 112.1(6) ?
C12 N1 Cd1 4_565 . 112.1(6) ?
C14 N1 Cd1 4_565 . 111.7(4) ?
C14 N1 Cd1 . . 111.7(4) ?
C11 N2 C13 4_565 . 129.5(9) ?
C11 N2 C13 . . 113.2(8) ?
C11 N2 C13 4_565 4_565 113.2(8) ?
C11 N2 C13 . 4_565 129.5(9) ?
C13 N2 C13 . 4_565 77.1(14) ?
C11 N2 C15 4_565 . 111.9(6) ?
C11 N2 C15 . . 92.3(6) ?
C13 N2 C15 4_565 . 98.6(9) ?
C11 N2 C15 4_565 4_565 92.3(6) ?
C11 N2 C15 . 4_565 111.9(6) ?
C13 N2 C15 . 4_565 98.6(9) ?
C15 N2 C15 . 4_565 117.7(9) ?
C11 N2 Cd1 4_565 1_554 111.0(4) ?
C11 N2 Cd1 . 1_554 111.0(4) ?
C13 N2 Cd1 . 1_554 110.3(7) ?
C13 N2 Cd1 4_565 1_554 110.3(7) ?
C15 N2 Cd1 . 1_554 111.3(4) ?
C15 N2 Cd1 4_565 1_554 111.3(4) ?
C9 O1 Cd1 . . 92.2(3) ?
C9 O2 Cd1 . . 93.3(3) ?
Cd1 O1W H1 . . 128.3 ?
C2 C1 C6 . . 118.6(5) ?
C2 C1 C7 . . 119.1(4) ?
C6 C1 C7 . . 122.3(5) ?
C1 C2 C3 . . 120.9(6) ?
C1 C2 H2 . . 119.5 ?
C3 C2 H2 . . 119.5 ?
C4 C3 C2 . . 119.2(6) ?
C4 C3 H3 . . 120.4 ?
C2 C3 H3 . . 120.4 ?
C5 C4 C3 . . 120.4(5) ?
C5 C4 H4 . . 119.8 ?
C3 C4 H4 . . 119.8 ?
C4 C5 C6 . . 120.8(6) ?
C4 C5 H5 . . 119.6 ?
C6 C5 H5 . . 119.6 ?
C5 C6 C1 . . 120.1(5) ?
C5 C6 H6 . . 120.0 ?
C1 C6 H6 . . 120.0 ?
C8 C7 C1 . . 126.9(4) ?
C8 C7 H7 . . 116.6 ?
C1 C7 H7 . . 116.6 ?
C7 C8 C9 . . 124.1(4) ?
C7 C8 H8 . . 117.9 ?
C9 C8 H8 . . 117.9 ?
O2 C9 O1 . . 120.2(4) ?
O2 C9 C8 . . 118.6(4) ?
O1 C9 C8 . . 121.2(4) ?
O2 C9 Cd1 . . 59.6(2) ?
O1 C9 Cd1 . . 60.6(2) ?
C8 C9 Cd1 . . 177.8(4) ?
N1 C10 C11 . . 110.8(7) ?
N1 C10 H10A . . 109.5 ?
C11 C10 H10A . . 109.5 ?
N1 C10 H10B . . 109.5 ?
C11 C10 H10B . . 109.5 ?
H10A C10 H10B . . 108.1 ?
N2 C11 C10 . . 112.3(6) ?
N2 C11 H11A . . 109.2 ?
C10 C11 H11A . . 109.2 ?
N2 C11 H11B . . 109.2 ?
C10 C11 H11B . . 109.2 ?
H11A C11 H11B . . 107.9 ?
N1 C12 C13 . . 109.7(10) ?
N1 C12 H12A . . 109.7 ?
C13 C12 H12A . . 109.7 ?
N1 C12 H12B . . 109.7 ?
C13 C12 H12B . . 109.7 ?
H12A C12 H12B . . 108.2 ?
N2 C13 C12 . . 110.4(12) ?
N2 C13 H13A . . 109.6 ?
C12 C13 H13A . . 109.6 ?
N2 C13 H13B . . 109.6 ?
C12 C13 H13B . . 109.6 ?
H13A C13 H13B . . 108.1 ?
N1 C14 C15 . . 111.2(7) ?
N1 C14 H14A . . 109.4 ?
C15 C14 H14A . . 109.4 ?
N1 C14 H14B . . 109.4 ?
C15 C14 H14B . . 109.4 ?
H14A C14 H14B . . 108.0 ?
N2 C15 C14 . . 110.6(7) ?
N2 C15 H15A . . 109.5 ?
C14 C15 H15A . . 109.5 ?
N2 C15 H15B . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 108.1 ?
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 O1W . 2.286(4) y
Cd1 O2 . 2.375(4) y
Cd1 O2 4_565 2.375(4) n
Cd1 O1 4_565 2.398(3) n
Cd1 O1 . 2.398(3) y
Cd1 N1 . 2.424(5) y
Cd1 N2 1_556 2.459(5) y
Cd1 C9 4_565 2.749(4) ?
Cd1 C9 . 2.749(4) ?
N1 C10 4_565 1.448(10) ?
N1 C10 . 1.448(10) ?
N1 C12 . 1.488(13) ?
N1 C12 4_565 1.488(13) ?
N1 C14 4_565 1.491(10) ?
N1 C14 . 1.491(10) ?
N2 C11 4_565 1.442(9) ?
N2 C11 . 1.442(9) ?
N2 C13 . 1.459(16) ?
N2 C13 4_565 1.459(16) ?
N2 C15 . 1.501(10) ?
N2 C15 4_565 1.501(10) ?
N2 Cd1 1_554 2.459(5) ?
O1 C9 . 1.257(6) ?
O2 C9 . 1.255(5) ?
O1W H1 . 0.8522 ?
C1 C2 . 1.379(7) ?
C1 C6 . 1.385(7) ?
C1 C7 . 1.472(6) ?
C2 C3 . 1.385(8) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.377(9) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.351(8) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.380(8) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.311(6) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.468(6) ?
C8 H8 . 0.9300 ?
C10 C11 . 1.542(12) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C12 C13 . 1.59(2) ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C13 H13A . 0.9700 ?
C13 H13B . 0.9700 ?
C14 C15 . 1.535(15) ?
C14 H14A . 0.9700 ?
C14 H14B . 0.9700 ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
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
O1W H1 O1 1_655 0.85 1.89 2.711(5) 162
