#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:49:32 +0300 (Fri, 06 May 2016) $
#$Revision: 182642 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/44/7224453.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_7224453
loop_
_publ_author_name
'Nawrot, I.'
'Machura, B.'
'Kruszynski, R.'
_publ_section_title
;
 Exploration of Cd(ii)/pseudohalide/di-2-pyridyl ketone chemistry --
 rational synthesis, structural analysis and photoluminescence
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2650
_journal_paper_doi               10.1039/C6CE00112B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C46 H40 Cd4 N16 O14'
_chemical_formula_sum            'C46 H40 Cd4 N16 O14'
_chemical_formula_weight         1490.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.398(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4664(6)
_cell_length_b                   12.4449(5)
_cell_length_c                   16.1614(7)
_cell_measurement_reflns_used    4439
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      28.3500
_cell_measurement_theta_min      3.9030
_cell_volume                     2664.0(2)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13051
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12453
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0376
_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)+(0.0399P)²+1.8030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                3736
_reflns_number_total             4731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00112b2.cif
_cod_data_source_block           cd135
_cod_depositor_comments
'Adding full bibliography for 7224447--7224455.cif.'
_cod_original_cell_volume        2664.00(19)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7224453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
C1 C 0.2442(4) -0.2538(5) 0.5094(3) 0.0574(13) Uani 1 1 d .
H1 H 0.2973 -0.3025 0.5203 0.069 Uiso 1 1 calc R
C2 C 0.1493(5) -0.2920(5) 0.4806(5) 0.085(2) Uani 1 1 d .
H2 H 0.1374 -0.3652 0.4722 0.102 Uiso 1 1 calc R
C3 C 0.0724(5) -0.2195(7) 0.4646(5) 0.105(3) Uani 1 1 d .
H3 H 0.0067 -0.2429 0.4454 0.126 Uiso 1 1 calc R
C4 C 0.0918(4) -0.1126(6) 0.4766(5) 0.0809(19) Uani 1 1 d .
H4 H 0.0395 -0.0629 0.4651 0.097 Uiso 1 1 calc R
C5 C 0.1880(4) -0.0786(4) 0.5056(3) 0.0502(13) Uani 1 1 d .
C6 C 0.2181(3) 0.0402(4) 0.5191(3) 0.0437(11) Uani 1 1 d .
C7 C 0.2227(4) 0.0726(4) 0.6130(4) 0.0547(14) Uani 1 1 d .
C8 C 0.1600(4) 0.0296(6) 0.6628(4) 0.0751(18) Uani 1 1 d .
H8 H 0.1133 -0.0232 0.6419 0.090 Uiso 1 1 calc R
C9 C 0.1673(7) 0.0655(8) 0.7433(5) 0.104(3) Uani 1 1 d .
H9 H 0.1259 0.0372 0.7781 0.125 Uiso 1 1 calc R
C10 C 0.2356(7) 0.1430(8) 0.7722(4) 0.107(3) Uani 1 1 d .
H10 H 0.2420 0.1675 0.8273 0.129 Uiso 1 1 calc R
C11 C 0.2950(5) 0.1849(6) 0.7199(4) 0.084(2) Uani 1 1 d .
H11 H 0.3406 0.2393 0.7395 0.101 Uiso 1 1 calc R
C12 C 0.1323(5) 0.1170(6) 0.3914(4) 0.083(2) Uani 1 1 d .
H12A H 0.1275 0.0472 0.3656 0.124 Uiso 1 1 calc R
H12B H 0.1920 0.1526 0.3808 0.124 Uiso 1 1 calc R
H12C H 0.0739 0.1587 0.3683 0.124 Uiso 1 1 calc R
C13 C 0.4079(5) -0.0803(5) 0.7568(4) 0.0759(19) Uani 1 1 d .
H13 H 0.3586 -0.1323 0.7406 0.091 Uiso 1 1 calc R
C14 C 0.4292(6) -0.0501(7) 0.8396(4) 0.091(2) Uani 1 1 d .
H14 H 0.3949 -0.0804 0.8788 0.109 Uiso 1 1 calc R
C15 C 0.5011(6) 0.0248(7) 0.8626(4) 0.091(2) Uani 1 1 d .
H15 H 0.5164 0.0469 0.9185 0.109 Uiso 1 1 calc R
C16 C 0.5520(5) 0.0687(5) 0.8049(3) 0.0682(17) Uani 1 1 d .
H16 H 0.6026 0.1193 0.8210 0.082 Uiso 1 1 calc R
C17 C 0.5262(4) 0.0360(4) 0.7209(3) 0.0488(12) Uani 1 1 d .
C18 C 0.5823(3) 0.0764(4) 0.6520(3) 0.0410(11) Uani 1 1 d .
C19 C 0.6149(4) 0.1942(4) 0.6659(3) 0.0475(12) Uani 1 1 d .
C20 C 0.7122(4) 0.2227(5) 0.7002(3) 0.0627(15) Uani 1 1 d .
H20 H 0.7606 0.1703 0.7182 0.075 Uiso 1 1 calc R
C21 C 0.7369(5) 0.3295(6) 0.7075(4) 0.0805(18) Uani 1 1 d .
H21 H 0.8026 0.3501 0.7300 0.097 Uiso 1 1 calc R
C22 C 0.6654(5) 0.4054(5) 0.6817(4) 0.0815(19) Uani 1 1 d .
H22 H 0.6812 0.4782 0.6865 0.098 Uiso 1 1 calc R
C23 C 0.5689(5) 0.3716(5) 0.6483(4) 0.0701(16) Uani 1 1 d .
H23 H 0.5196 0.4230 0.6303 0.084 Uiso 1 1 calc R
N1 N 0.2639(3) -0.1497(3) 0.5227(2) 0.0471(10) Uani 1 1 d .
N2 N 0.2885(3) 0.1487(4) 0.6401(3) 0.0588(12) Uani 1 1 d .
N3 N 0.4556(3) -0.0377(4) 0.6977(2) 0.0532(11) Uani 1 1 d .
N4 N 0.5436(3) 0.2672(3) 0.6410(2) 0.0535(11) Uani 1 1 d .
N5 N 0.2688(5) 0.3988(5) 0.5186(4) 0.0830(17) Uani 1 1 d .
N97 N 0.5502(5) -0.3405(6) 0.6809(4) 0.111(2) Uani 1 1 d .
N98 N 0.5344(3) -0.2860(4) 0.6225(3) 0.0602(12) Uani 1 1 d .
N99 N 0.5176(3) -0.2302(4) 0.5630(3) 0.0569(11) Uani 1 1 d .
O1 O 0.3078(2) 0.0587(2) 0.49455(18) 0.0393(7) Uani 1 1 d .
O2 O 0.1374(2) 0.1059(3) 0.4779(2) 0.0569(9) Uani 1 1 d .
O3 O 0.5212(2) 0.0686(2) 0.57369(17) 0.0340(7) Uani 1 1 d .
O4 O 0.6685(2) 0.0109(3) 0.65970(19) 0.0503(9) Uani 1 1 d .
H4A H 0.6741 -0.0122 0.6133 0.076 Uiso 1 1 calc R
O5 O 0.3350(5) 0.3842(5) 0.5795(4) 0.1200(19) Uani 1 1 d .
O6 O 0.2676(5) 0.3293(5) 0.4652(4) 0.128(2) Uani 1 1 d .
O7 O 0.2131(6) 0.4715(6) 0.5107(4) 0.173(3) Uani 1 1 d .
Cd1 Cd 0.42325(2) -0.07830(3) 0.55349(2) 0.03811(12) Uani 1 1 d .
Cd2 Cd 0.39638(3) 0.20845(3) 0.54745(2) 0.04532(13) Uani 1 1 d .
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'
Cd Cd -0.8075 1.2024 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 122.8(5) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C2 C1 117.8(6) . .
C3 C2 H2 121.1 . .
C1 C2 H2 121.1 . .
C2 C3 C4 120.0(6) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 C5 119.8(6) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
N1 C5 C4 120.5(5) . .
N1 C5 C6 115.7(4) . .
C4 C5 C6 123.8(5) . .
O1 C6 O2 114.1(4) . .
O1 C6 C5 110.3(4) . .
O2 C6 C5 109.0(4) . .
O1 C6 C7 111.0(4) . .
O2 C6 C7 101.6(3) . .
C5 C6 C7 110.5(4) . .
N2 C7 C8 122.2(6) . .
N2 C7 C6 114.6(4) . .
C8 C7 C6 123.2(6) . .
C9 C8 C7 119.0(7) . .
C9 C8 H8 120.5 . .
C7 C8 H8 120.5 . .
C10 C9 C8 119.4(7) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C11 119.6(7) . .
C9 C10 H10 120.2 . .
C11 C10 H10 120.2 . .
N2 C11 C10 121.2(8) . .
N2 C11 H11 119.4 . .
C10 C11 H11 119.4 . .
O2 C12 H12A 109.5 . .
O2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
O2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 C14 122.7(7) . .
N3 C13 H13 118.6 . .
C14 C13 H13 118.6 . .
C15 C14 C13 118.3(6) . .
C15 C14 H14 120.9 . .
C13 C14 H14 120.9 . .
C14 C15 C16 120.7(6) . .
C14 C15 H15 119.6 . .
C16 C15 H15 119.6 . .
C15 C16 C17 118.6(7) . .
C15 C16 H16 120.7 . .
C17 C16 H16 120.7 . .
N3 C17 C16 121.1(5) . .
N3 C17 C18 116.2(4) . .
C16 C17 C18 122.6(5) . .
O3 C18 O4 112.7(3) . .
O3 C18 C19 108.0(4) . .
O4 C18 C19 109.4(4) . .
O3 C18 C17 110.5(4) . .
O4 C18 C17 104.5(4) . .
C19 C18 C17 111.8(4) . .
N4 C19 C20 122.0(5) . .
N4 C19 C18 115.9(4) . .
C20 C19 C18 122.1(5) . .
C21 C20 C19 118.9(6) . .
C21 C20 H20 120.5 . .
C19 C20 H20 120.5 . .
C22 C21 C20 120.0(6) . .
C22 C21 H21 120.0 . .
C20 C21 H21 120.0 . .
C21 C22 C23 118.2(6) . .
C21 C22 H22 120.9 . .
C23 C22 H22 120.9 . .
N4 C23 C22 122.4(6) . .
N4 C23 H23 118.8 . .
C22 C23 H23 118.8 . .
C1 N1 C5 119.0(4) . .
C1 N1 Cd1 124.3(3) . .
C5 N1 Cd1 115.9(3) . .
C7 N2 C11 118.7(5) . .
C7 N2 Cd2 117.7(3) . .
C11 N2 Cd2 123.5(5) . .
C17 N3 C13 118.6(5) . .
C17 N3 Cd1 115.2(3) . .
C13 N3 Cd1 126.2(4) . .
C19 N4 C23 118.4(5) . .
C19 N4 Cd2 117.1(3) . .
C23 N4 Cd2 121.5(4) . .
O7 N5 O5 124.6(8) . .
O7 N5 O6 123.0(8) . .
O5 N5 O6 112.4(6) . .
N97 N98 N99 179.5(6) . .
N98 N99 Cd1 124.8(4) . .
N98 N99 Cd2 130.7(4) . 3_656
Cd1 N99 Cd2 101.69(17) . 3_656
C6 O1 Cd2 117.3(3) . .
C6 O1 Cd1 108.2(3) . .
Cd2 O1 Cd1 100.04(11) . .
C12 O2 C6 115.0(4) . .
C18 O3 Cd1 115.3(3) . .
C18 O3 Cd1 125.1(3) . 3_656
Cd1 O3 Cd1 100.91(10) . 3_656
C18 O3 Cd2 113.1(2) . .
Cd1 O3 Cd2 100.95(10) . .
Cd1 O3 Cd2 97.66(10) 3_656 .
C18 O4 H4A 109.5 . .
N5 O5 Cd2 101.0(4) . .
N5 O6 Cd2 97.5(4) . .
O3 Cd1 N99 111.23(14) . .
O3 Cd1 N1 148.25(12) . .
N99 Cd1 N1 100.49(16) . .
O3 Cd1 O3 79.09(10) . 3_656
N99 Cd1 O3 80.61(13) . 3_656
N1 Cd1 O3 105.49(12) . 3_656
O3 Cd1 N3 71.43(13) . .
N99 Cd1 N3 96.38(15) . .
N1 Cd1 N3 107.31(14) . .
O3 Cd1 N3 147.05(13) 3_656 .
O3 Cd1 O1 78.44(10) . .
N99 Cd1 O1 159.91(14) . .
N1 Cd1 O1 70.96(12) . .
O3 Cd1 O1 84.24(9) 3_656 .
N3 Cd1 O1 103.49(12) . .
O1 Cd2 N99 96.14(13) . 3_656
O1 Cd2 N4 143.48(13) . .
N99 Cd2 N4 88.75(15) 3_656 .
O1 Cd2 N2 69.26(14) . .
N99 Cd2 N2 165.39(16) 3_656 .
N4 Cd2 N2 103.22(15) . .
O1 Cd2 O3 77.13(10) . .
N99 Cd2 O3 77.82(12) 3_656 .
N4 Cd2 O3 68.57(12) . .
N2 Cd2 O3 98.57(12) . .
O1 Cd2 O5 129.64(17) . .
N99 Cd2 O5 107.24(19) 3_656 .
N4 Cd2 O5 82.20(18) . .
N2 Cd2 O5 82.98(19) . .
O3 Cd2 O5 150.36(17) . .
O1 Cd2 O6 91.52(18) . .
N99 Cd2 O6 85.14(18) 3_656 .
N4 Cd2 O6 125.0(2) . .
N2 Cd2 O6 94.52(18) . .
O3 Cd2 O6 158.25(17) . .
O5 Cd2 O6 48.6(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.332(7) .
C1 C2 1.364(8) .
C1 H1 0.9300 .
C2 C3 1.363(9) .
C2 H2 0.9300 .
C3 C4 1.363(9) .
C3 H3 0.9300 .
C4 C5 1.363(7) .
C4 H4 0.9300 .
C5 N1 1.343(6) .
C5 C6 1.538(7) .
C6 O1 1.358(5) .
C6 O2 1.425(5) .
C6 C7 1.560(7) .
C7 N2 1.316(7) .
C7 C8 1.376(7) .
C8 C9 1.362(10) .
C8 H8 0.9300 .
C9 C10 1.356(11) .
C9 H9 0.9300 .
C10 C11 1.368(10) .
C10 H10 0.9300 .
C11 N2 1.355(7) .
C11 H11 0.9300 .
C12 O2 1.393(7) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 N3 1.351(7) .
C13 C14 1.370(9) .
C13 H13 0.9300 .
C14 C15 1.347(10) .
C14 H14 0.9300 .
C15 C16 1.367(9) .
C15 H15 0.9300 .
C16 C17 1.399(7) .
C16 H16 0.9300 .
C17 N3 1.326(7) .
C17 C18 1.540(7) .
C18 O3 1.382(5) .
C18 O4 1.406(5) .
C18 C19 1.535(7) .
C19 N4 1.330(6) .
C19 C20 1.375(7) .
C20 C21 1.371(8) .
C20 H20 0.9300 .
C21 C22 1.359(9) .
C21 H21 0.9300 .
C22 C23 1.380(9) .
C22 H22 0.9300 .
C23 N4 1.344(7) .
C23 H23 0.9300 .
N1 Cd1 2.293(4) .
N2 Cd2 2.385(4) .
N3 Cd1 2.347(4) .
N4 Cd2 2.381(4) .
N5 O7 1.167(7) .
N5 O5 1.216(7) .
N5 O6 1.220(7) .
N97 N98 1.151(7) .
N98 N99 1.174(6) .
N99 Cd1 2.268(4) .
N99 Cd2 2.313(4) 3_656
O1 Cd2 2.293(3) .
O1 Cd1 2.386(3) .
O3 Cd1 2.243(3) .
O3 Cd1 2.314(3) 3_656
O3 Cd2 2.404(3) .
O4 H4A 0.8200 .
O5 Cd2 2.427(5) .
O6 Cd2 2.491(6) .
Cd1 O3 2.314(3) 3_656
Cd2 N99 2.313(4) 3_656
