#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/63/2016312.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_2016312
loop_
_publ_author_name
'Tafeenko, Viktor A.'
'Panin, Gennady N. '
'Baranov, Andrey N. '
'Bardasov, Ivan N.'
'Aslanov, Leonid A.'
_publ_section_title
;
 Luminescent properties of three structures built from
 3-cyano-4-dicyanomethylene-5-oxo-4,5-dihydro-1H-pyrrol-2-olate
 and cadmium
;
_journal_coeditor_code           GA3063
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m541
_journal_page_last               m547
_journal_paper_doi               10.1107/S0108270107045453
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cd (C8 H1 N4 O2)2 (H2 O1)4], 2H2 O'
_chemical_formula_moiety         'C16 H10 Cd N8 O8, 2(H2 O)'
_chemical_formula_sum            'C16 H14 Cd N8 O10'
_chemical_formula_weight         590.76
_chemical_melting_point          190
_chemical_name_systematic
;
tetraaquabis(3-cyano-4-dicyanomethylene-5-oxo-4,5-dihydro-1H-pyrrol-2-\
olato)cadmium(II) dihydrate
;
_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                105.48(2)
_cell_angle_beta                 97.08(2)
_cell_angle_gamma                110.28(3)
_cell_formula_units_Z            1
_cell_length_a                   6.987(2)
_cell_length_b                   8.645(2)
_cell_length_c                   10.567(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      14
_cell_volume                     560.3(3)
_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_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4 diffractometr'
_diffrn_measurement_method       'non-profiled omega scan'
_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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2838
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.9027
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0363P)²+0.2027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                2503
_reflns_number_total             2693
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ga3063.cif
_cod_data_source_block           I
_cod_database_code               2016312
_cod_database_fobs_code          2016312
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.5000 1.0000 0.03556(10) Uani d S 1
O O1 0.5587(3) 0.9360(2) 0.64762(17) 0.0408(4) Uani d . 1
O O2 0.0764(3) 0.5289(3) 0.26638(17) 0.0439(4) Uani d . 1
O O3 0.1451(3) 0.3930(3) 0.9348(2) 0.0603(6) Uani d D 1
H H3 0.0939 0.3115 0.9626 0.090 Uiso calc RD 1
H H31 0.0783 0.4154 0.8818 0.090 Uiso d RD 1
O O4 0.5013(4) 0.7512(3) 1.1319(2) 0.0663(7) Uani d D 1
H H4 0.4237 0.7822 1.0894 0.099 Uiso calc RD 1
H H41 0.6063 0.8321 1.1955 0.099 Uiso d RD 1
O O5 0.2138(5) 0.8888(3) 1.0657(2) 0.0657(6) Uani d D 1
H H51 0.208 0.909 0.993 0.099 Uiso d RD 1
H H5 0.251 0.981 1.130 0.099 Uiso d RD 1
N N1 0.3211(3) 0.7656(3) 0.4415(2) 0.0347(4) Uani d . 1
H H1 0.3319 0.8465 0.4066 0.042 Uiso calc R 1
N N2 0.1956(4) 0.1716(3) 0.6116(3) 0.0551(7) Uani d . 1
N N3 -0.1005(5) 0.1132(4) 0.2058(3) 0.0704(9) Uani d . 1
N N4 0.5019(4) 0.5979(3) 0.8151(2) 0.0461(6) Uani d . 1
C C2 0.4311(4) 0.7943(3) 0.5707(2) 0.0303(5) Uani d . 1
C C3 0.3646(3) 0.6266(3) 0.5914(2) 0.0277(4) Uani d . 1
C C4 0.2261(3) 0.4979(3) 0.4741(2) 0.0263(4) Uani d . 1
C C5 0.1943(4) 0.5933(3) 0.3774(2) 0.0309(5) Uani d . 1
C C6 0.1291(4) 0.3193(3) 0.4400(2) 0.0300(5) Uani d . 1
C C7 0.0020(4) 0.2080(3) 0.3089(3) 0.0413(6) Uani d . 1
C C8 0.1637(4) 0.2352(3) 0.5346(3) 0.0352(5) Uani d . 1
C C9 0.4397(4) 0.6098(3) 0.7143(2) 0.0314(5) 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'
Cd Cd -0.8075 1.2024 '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'
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
O4 Cd1 O4 2_667 . 180.0000(10) ?
O4 Cd1 O3 2_667 2_667 89.47(10) ?
O4 Cd1 O3 . 2_667 90.53(10) ?
O4 Cd1 O3 2_667 . 90.53(10) ?
O4 Cd1 O3 . . 89.47(10) y
O3 Cd1 O3 2_667 . 180.0 ?
O4 Cd1 N4 2_667 2_667 90.89(9) ?
O4 Cd1 N4 . 2_667 89.11(9) ?
O3 Cd1 N4 2_667 2_667 86.31(9) ?
O3 Cd1 N4 . 2_667 93.69(9) ?
O4 Cd1 N4 2_667 . 89.11(9) ?
O4 Cd1 N4 . . 90.89(9) y
O3 Cd1 N4 2_667 . 93.69(9) ?
O3 Cd1 N4 . . 86.31(9) y
N4 Cd1 N4 2_667 . 180.0000(10) ?
Cd1 O3 H3 . . 109.5 ?
Cd1 O3 H31 . . 126.6 ?
H3 O3 H31 . . 122.9 ?
Cd1 O4 H4 . . 109.5 ?
Cd1 O4 H41 . . 125.6 ?
H4 O4 H41 . . 117.4 ?
H51 O5 H5 . . 110.4 ?
C5 N1 C2 . . 111.62(19) ?
C5 N1 H1 . . 124.2 ?
C2 N1 H1 . . 124.2 ?
C9 N4 Cd1 . . 158.7(2) ?
O1 C2 N1 . . 124.7(2) ?
O1 C2 C3 . . 128.6(2) ?
N1 C2 C3 . . 106.7(2) ?
C4 C3 C9 . . 129.0(2) ?
C4 C3 C2 . . 109.39(19) ?
C9 C3 C2 . . 121.6(2) ?
C6 C4 C3 . . 132.0(2) ?
C6 C4 C5 . . 122.4(2) ?
C3 C4 C5 . . 105.64(19) ?
O2 C5 N1 . . 127.1(2) ?
O2 C5 C4 . . 126.4(2) ?
N1 C5 C4 . . 106.53(18) ?
C4 C6 C7 . . 123.1(2) ?
C4 C6 C8 . . 120.4(2) ?
C7 C6 C8 . . 116.4(2) ?
N3 C7 C6 . . 177.2(3) ?
N2 C8 C6 . . 178.4(3) ?
N4 C9 C3 . . 179.3(3) ?
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 O4 2_667 2.242(2) ?
Cd1 O4 . 2.242(2) y
Cd1 O3 2_667 2.264(2) ?
Cd1 O3 . 2.264(2) y
Cd1 N4 2_667 2.327(2) ?
Cd1 N4 . 2.327(2) y
O1 C2 . 1.220(3) ?
O2 C5 . 1.208(3) ?
O3 H3 . 0.8200 ?
O3 H31 . 0.7907 ?
O4 H4 . 0.8200 ?
O4 H41 . 0.8665 ?
O5 H51 . 0.83 ?
O5 H5 . 0.83 ?
N1 C5 . 1.365(3) ?
N1 C2 . 1.394(3) ?
N1 H1 . 0.8600 ?
N2 C8 . 1.137(3) ?
N3 C7 . 1.139(4) ?
N4 C9 . 1.144(3) ?
C2 C3 . 1.446(3) ?
C3 C4 . 1.390(3) ?
C3 C9 . 1.404(3) ?
C4 C6 . 1.374(3) ?
C4 C5 . 1.515(3) ?
C6 C7 . 1.423(3) ?
C6 C8 . 1.428(3) ?
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
N1 H1 O1 2_676 0.86 2.03 2.870(3) 164.2
O4 H4 O5 . 0.82 2.01 2.773(4) 155.2
O3 H31 O2 2_566 0.79 2.05 2.837(3) 174.8
O5 H51 N3 2_566 0.83 2.08 2.874(4) 161
O3 H3 O5 2_567 0.82 2.17 2.825(4) 137.3
O5 H5 O1 2_677 0.83 2.34 2.949(3) 131
O4 H41 N2 2_667 0.87 2.33 2.986(3) 132.3
