#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:54:31 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244069 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/81/7238103.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_7238103
loop_
_publ_author_name
'Zhang, Hong-Tao'
'Li, Yi-Zhi'
'Wang, Hua-Qin'
'Nfor, Emmanuel N.'
'You, Xiao-Zeng'
_publ_section_title
;
 From loop-like chain to helix: a result of symmetry breaking triggered by
 the replacement of coordination water
;
_journal_issue                   94
_journal_name_full               CrystEngComm
_journal_page_first              578
_journal_paper_doi               10.1039/b510446g
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C11 H9 Cd N3 O7, H2 O'
_chemical_formula_sum            'C11 H11 Cd N3 O8'
_chemical_formula_weight         425.63
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                117.25(3)
_cell_angle_beta                 104.93(3)
_cell_angle_gamma                98.44(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1420(18)
_cell_length_b                   9.5970(19)
_cell_length_c                   9.904(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.4
_cell_volume                     710.1(4)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'ω 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2924
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         18
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XCAD4 (Harms & Wocadlo, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0325
_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)+(0.0506P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2346
_reflns_number_total             2741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b510446g.txt
_cod_data_source_block           cd
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238103
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_calc_flag
_atom_site_refinement_flags
Cd Cd 0.97798(3) 0.31026(3) 0.53249(3) 0.03052(12) Uani 1 1 d .
O5 O 0.4739(4) 0.0125(4) -0.2844(5) 0.0634(10) Uani 1 1 d .
O6 O 0.4332(5) -0.2305(6) -0.4853(4) 0.0742(13) Uani 1 1 d .
N1 N 0.5050(4) -0.1167(5) -0.3448(5) 0.0418(9) Uani 1 1 d .
C1 C 0.8652(5) 0.0617(4) 0.2120(5) 0.0293(8) Uani 1 1 d .
C2 C 0.8033(4) -0.0553(4) 0.0299(4) 0.0253(7) Uani 1 1 d .
C3 C 0.6850(5) -0.0329(5) -0.0707(5) 0.0294(8) Uani 1 1 d .
H3 H 0.6418 0.0518 -0.0268 0.035 Uiso 1 1 calc R
C4 C 0.6327(4) -0.1389(5) -0.2376(5) 0.0289(8) Uani 1 1 d .
O2 O 0.8134(4) 0.1819(3) 0.2650(3) 0.0415(7) Uani 1 1 d .
O1 O 0.9696(4) 0.0395(4) 0.3040(3) 0.0408(7) Uani 1 1 d .
O7 O 0.8681(4) 0.1421(4) 0.6132(4) 0.0468(8) Uani 1 1 d .
H2A H 0.9116 0.0520 0.5872 0.070 Uiso 1 1 d R
H2B H 0.7548 0.1001 0.5564 0.070 Uiso 1 1 d R
C7 C 0.8679(4) -0.1811(4) -0.0385(4) 0.0240(7) Uani 1 1 d .
H7 H 0.9466 -0.1966 0.0294 0.029 Uiso 1 1 calc R
C6 C 0.8164(4) -0.2841(4) -0.2072(4) 0.0241(7) Uani 1 1 d .
C5 C 0.6956(4) -0.2644(5) -0.3101(4) 0.0279(8) Uani 1 1 d .
H5 H 0.6587 -0.3331 -0.4230 0.033 Uiso 1 1 calc R
O3 O 0.9572(4) -0.4697(4) -0.1937(4) 0.0403(7) Uani 1 1 d .
O4 O 0.8738(3) -0.4779(3) -0.4275(3) 0.0325(6) Uani 1 1 d .
C8 C 0.8880(4) -0.4182(4) -0.2798(4) 0.0257(7) Uani 1 1 d .
N2 N 1.2294(4) 0.3685(4) 0.6784(4) 0.0316(7) Uani 1 1 d .
C9 C 1.3105(5) 0.2697(5) 0.6934(5) 0.0348(9) Uani 1 1 d .
H9 H 1.2667 0.1569 0.6471 0.042 Uiso 1 1 calc R
C10 C 1.3364(5) 0.5228(5) 0.7647(5) 0.0378(9) Uani 1 1 d .
H10 H 1.3130 0.6179 0.7765 0.045 Uiso 1 1 calc R
N3 N 1.4627(4) 0.3536(5) 0.7836(4) 0.0408(8) Uani 1 1 d .
H1 H 1.5364 0.3136 0.8085 0.049 Uiso 1 1 calc R
C11 C 1.4817(5) 0.5149(6) 0.8302(6) 0.0437(11) Uani 1 1 d .
H11 H 1.5761 0.6020 0.8942 0.052 Uiso 1 1 calc R
O8 O 0.7824(4) 0.3409(5) 0.8901(4) 0.0538(9) Uani 1 1 d .
H4B H 0.8398 0.2965 0.9296 0.081 Uiso 1 1 d R
H4A H 0.8162 0.4448 0.9548 0.081 Uiso 1 1 d R
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Cd O2 139.30(12) . .
N2 Cd O4 118.65(12) . 1_566
O2 Cd O4 86.17(10) . 1_566
N2 Cd O7 97.48(12) . .
O2 Cd O7 101.31(12) . .
O4 Cd O7 113.20(11) 1_566 .
N2 Cd O1 93.59(12) . .
O2 Cd O1 54.20(10) . .
O4 Cd O1 140.12(10) 1_566 .
O7 Cd O1 82.41(11) . .
N2 Cd O3 86.66(12) . 1_566
O2 Cd O3 132.21(10) . 1_566
O4 Cd O3 52.49(9) 1_566 1_566
O7 Cd O3 78.83(11) . 1_566
O1 Cd O3 161.10(10) . 1_566
N2 Cd C1 117.09(13) . .
O2 Cd C1 26.98(11) . .
O4 Cd C1 112.95(11) 1_566 .
O7 Cd C1 92.96(12) . .
O1 Cd C1 27.25(11) . .
O3 Cd C1 155.86(11) 1_566 .
O6 N1 O5 124.3(4) . .
O6 N1 C4 118.2(4) . .
O5 N1 C4 117.4(4) . .
O2 C1 O1 122.5(4) . .
O2 C1 C2 117.7(3) . .
O1 C1 C2 119.7(3) . .
O2 C1 Cd 55.9(2) . .
O1 C1 Cd 66.7(2) . .
C2 C1 Cd 171.5(3) . .
C3 C2 C7 119.8(3) . .
C3 C2 C1 119.5(3) . .
C7 C2 C1 120.7(3) . .
C4 C3 C2 118.6(3) . .
C4 C3 H3 120.7 . .
C2 C3 H3 120.7 . .
C3 C4 C5 123.2(3) . .
C3 C4 N1 118.6(3) . .
C5 C4 N1 118.1(3) . .
C1 O2 Cd 97.1(2) . .
C1 O1 Cd 86.0(2) . .
Cd O7 H2A 109.3 . .
Cd O7 H2B 109.3 . .
H2A O7 H2B 109.5 . .
C2 C7 C6 120.8(3) . .
C2 C7 H7 119.6 . .
C6 C7 H7 119.6 . .
C7 C6 C5 120.1(3) . .
C7 C6 C8 120.4(3) . .
C5 C6 C8 119.5(3) . .
C4 C5 C6 117.5(3) . .
C4 C5 H5 121.2 . .
C6 C5 H5 121.2 . .
C8 O3 Cd 84.3(2) . 1_544
C8 O4 Cd 100.8(2) . 1_544
O3 C8 O4 122.1(3) . .
O3 C8 C6 119.2(3) . .
O4 C8 C6 118.6(3) . .
C9 N2 C10 106.3(3) . .
C9 N2 Cd 130.0(3) . .
C10 N2 Cd 123.6(3) . .
N2 C9 N3 110.6(4) . .
N2 C9 H9 124.7 . .
N3 C9 H9 124.7 . .
C11 C10 N2 108.9(4) . .
C11 C10 H10 125.5 . .
N2 C10 H10 125.5 . .
C9 N3 C11 107.9(4) . .
C9 N3 H1 126.0 . .
C11 N3 H1 126.0 . .
C10 C11 N3 106.3(4) . .
C10 C11 H11 126.9 . .
N3 C11 H11 126.9 . .
H4B O8 H4A 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd N2 2.204(3) .
Cd O2 2.283(3) .
Cd O4 2.286(3) 1_566
Cd O7 2.317(3) .
Cd O1 2.519(3) .
Cd O3 2.643(3) 1_566
Cd O4 2.669(3) 2_755
O5 N1 1.220(5) .
O6 N1 1.219(5) .
N1 C4 1.476(5) .
C1 O2 1.251(5) .
C1 O1 1.256(5) .
C1 C2 1.506(5) .
C2 C3 1.384(5) .
C2 C7 1.390(5) .
C3 C4 1.380(6) .
C3 H3 0.9300 .
C4 C5 1.386(5) .
O7 H2A 0.9600 .
O7 H2B 0.9600 .
C7 C6 1.392(5) .
C7 H7 0.9300 .
C6 C5 1.397(5) .
C6 C8 1.498(5) .
C5 H5 0.9300 .
O3 C8 1.254(5) .
O3 Cd 2.643(3) 1_544
O4 C8 1.263(4) .
O4 Cd 2.286(3) 1_544
N2 C9 1.323(5) .
N2 C10 1.366(5) .
C9 N3 1.324(6) .
C9 H9 0.9300 .
C10 C11 1.350(6) .
C10 H10 0.9300 .
N3 C11 1.366(6) .
N3 H1 0.8600 .
C11 H11 0.9300 .
O8 H4B 0.8500 .
O8 H4A 0.8500 .
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
N3 H1 O5 0.86 2.52 3.049(5) 120.9 1_656
N3 H1 O8 0.86 2.12 2.881(5) 148.1 1_655
O7 H2A O1 0.96 1.91 2.711(4) 139.1 2_756
O7 H2B O5 0.96 2.56 3.398(5) 145.6 2_655
O7 H2B O6 0.96 2.42 3.128(5) 130.8 2_655
O8 H4A O3 0.85 2.50 2.786(5) 100.3 1_566
O8 H4B O3 0.85 2.38 2.878(5) 118.0 2_756
O8 H4B O3 0.85 2.38 2.878(5) 118.0 2_756
