#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:49:32 +0300 (Fri, 06 May 2016) $
#$Revision: 182642 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/44/7224449.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_7224449
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         'C48 H44 Cd4 N20 O8'
_chemical_formula_sum            'C48 H44 Cd4 N20 O8'
_chemical_formula_weight         1478.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4180(5)
_cell_length_b                   18.4180(5)
_cell_length_c                   30.698(2)
_cell_measurement_reflns_used    4764
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      29.0740
_cell_measurement_theta_min      3.7310
_cell_volume                     10413.5(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            12961
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0384
_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)+(0.0415P)²+55.7509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                1616
_reflns_number_total             2298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00112b2.cif
_cod_data_source_block           cd126
_cod_depositor_comments
'Adding full bibliography for 7224447--7224455.cif.'
_cod_original_cell_volume        10413.6(8)
_cod_original_sg_symbol_H-M      I41/acd
_cod_database_code               7224449
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'y+3/4, x+1/4, -z+1/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-y-3/4, -x-1/4, z-1/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/4'
'y+1/4, x+1/4, z+1/4'
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 0.5478(3) 0.3306(3) -0.0201(2) 0.0350(14) Uani 1 1 d .
H1 H 0.5154 0.3693 -0.0208 0.042 Uiso 1 1 calc R
C2 C 0.5735(3) 0.3042(4) -0.0590(2) 0.0406(16) Uani 1 1 d .
H2 H 0.5579 0.3236 -0.0854 0.049 Uiso 1 1 calc R
C3 C 0.6228(4) 0.2485(4) -0.0579(2) 0.0440(17) Uani 1 1 d .
H3 H 0.6414 0.2296 -0.0836 0.053 Uiso 1 1 calc R
C4 C 0.6443(3) 0.2209(3) -0.0186(2) 0.0369(15) Uani 1 1 d .
H4 H 0.6781 0.1834 -0.0176 0.044 Uiso 1 1 calc R
C5 C 0.6157(3) 0.2491(3) 0.0196(2) 0.0333(14) Uani 1 1 d .
C6 C 0.6368(3) 0.2213(3) 0.06514(19) 0.0252(13) Uani 1 1 d .
C7 C 0.3499(3) 0.3616(3) 0.06326(19) 0.0293(13) Uani 1 1 d .
C8 C 0.2824(3) 0.3940(3) 0.0675(2) 0.0364(15) Uani 1 1 d .
H8 H 0.2414 0.3666 0.0741 0.044 Uiso 1 1 calc R
C9 C 0.2775(4) 0.4681(3) 0.0617(3) 0.0522(19) Uani 1 1 d .
H9 H 0.2331 0.4915 0.0651 0.063 Uiso 1 1 calc R
C10 C 0.3381(4) 0.5068(4) 0.0510(3) 0.065(2) Uani 1 1 d .
H10 H 0.3350 0.5562 0.0453 0.078 Uiso 1 1 calc R
C11 C 0.4032(4) 0.4716(3) 0.0490(3) 0.052(2) Uani 1 1 d .
H11 H 0.4446 0.4988 0.0429 0.063 Uiso 1 1 calc R
C12 C 0.7114(3) 0.3257(3) 0.0790(2) 0.0454(17) Uani 1 1 d .
H12A H 0.7142 0.3435 0.0497 0.068 Uiso 1 1 calc R
H12B H 0.7545 0.3394 0.0946 0.068 Uiso 1 1 calc R
H12C H 0.6696 0.3462 0.0931 0.068 Uiso 1 1 calc R
N1 N 0.5669(2) 0.3034(2) 0.01872(16) 0.0290(11) Uani 1 1 d .
N2 N 0.4105(3) 0.4002(2) 0.05519(18) 0.0376(13) Uani 1 1 d .
N97 N 0.5615(5) 0.5700(3) 0.0883(2) 0.082(2) Uani 1 1 d .
N98 N 0.5711(3) 0.5099(3) 0.08057(18) 0.0450(14) Uani 1 1 d .
N99 N 0.5830(3) 0.4494(3) 0.0717(2) 0.0544(17) Uani 1 1 d .
O1 O 0.58278(19) 0.23619(19) 0.09476(12) 0.0266(9) Uani 1 1 d .
O2 O 0.7054(2) 0.2495(2) 0.07848(14) 0.0352(10) Uani 1 1 d .
Cd1 Cd 0.51870(2) 0.34733(2) 0.082667(14) 0.02593(16) 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 123.4(6) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C3 C2 C1 118.2(6) . .
C3 C2 H2 120.9 . .
C1 C2 H2 120.9 . .
C4 C3 C2 119.6(6) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C3 C4 C5 119.7(6) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N1 C5 C4 121.0(6) . .
N1 C5 C6 115.8(5) . .
C4 C5 C6 123.2(5) . .
O1 C6 O2 112.2(4) . .
O1 C6 C5 110.5(4) . .
O2 C6 C5 111.4(4) . .
O1 C6 C7 109.6(4) . 3_655
O2 C6 C7 103.3(4) . 3_655
C5 C6 C7 109.5(5) . 3_655
N2 C7 C8 122.3(5) . .
N2 C7 C6 113.4(5) . 3_655
C8 C7 C6 124.3(5) . 3_655
C9 C8 C7 118.2(6) . .
C9 C8 H8 120.9 . .
C7 C8 H8 120.9 . .
C10 C9 C8 119.7(6) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
C9 C10 C11 118.9(6) . .
C9 C10 H10 120.6 . .
C11 C10 H10 120.6 . .
N2 C11 C10 123.2(6) . .
N2 C11 H11 118.4 . .
C10 C11 H11 118.4 . .
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 . .
C1 N1 C5 118.1(5) . .
C1 N1 Cd1 121.8(4) . .
C5 N1 Cd1 120.1(4) . .
C11 N2 C7 117.6(5) . .
C11 N2 Cd1 122.6(4) . .
C7 N2 Cd1 114.5(4) . .
N97 N98 N99 177.5(8) . .
N98 N99 Cd1 131.6(5) . .
C6 O1 Cd1 124.2(3) . 26_565
C6 O1 Cd1 115.1(3) . .
Cd1 O1 Cd1 104.31(14) 26_565 .
C6 O1 Cd1 109.1(3) . 3_655
Cd1 O1 Cd1 102.49(14) 26_565 3_655
Cd1 O1 Cd1 97.90(13) . 3_655
C12 O2 C6 115.8(4) . .
O1 Cd1 N99 105.6(2) 20_656 .
O1 Cd1 N1 145.06(14) 20_656 .
N99 Cd1 N1 87.87(19) . .
O1 Cd1 N2 111.59(16) 20_656 .
N99 Cd1 N2 92.64(19) . .
N1 Cd1 N2 99.51(18) . .
O1 Cd1 O1 76.33(14) 20_656 .
N99 Cd1 O1 118.63(17) . .
N1 Cd1 O1 68.98(14) . .
N2 Cd1 O1 145.16(14) . .
O1 Cd1 O1 75.17(13) 20_656 3_655
N99 Cd1 O1 161.88(16) . 3_655
N1 Cd1 O1 101.74(14) . 3_655
N2 Cd1 O1 70.78(14) . 3_655
O1 Cd1 O1 79.37(13) . 3_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.341(7) .
C1 C2 1.372(9) .
C1 H1 0.9300 .
C2 C3 1.369(9) .
C2 H2 0.9300 .
C3 C4 1.366(9) .
C3 H3 0.9300 .
C4 C5 1.388(8) .
C4 H4 0.9300 .
C5 N1 1.344(7) .
C5 C6 1.539(9) .
C6 O1 1.376(6) .
C6 O2 1.425(6) .
C6 C7 1.547(7) 3_655
C7 N2 1.346(7) .
C7 C8 1.386(8) .
C7 C6 1.547(7) 3_655
C8 C9 1.379(8) .
C8 H8 0.9300 .
C9 C10 1.363(9) .
C9 H9 0.9300 .
C10 C11 1.365(9) .
C10 H10 0.9300 .
C11 N2 1.336(7) .
C11 H11 0.9300 .
C12 O2 1.409(7) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
N1 Cd1 2.301(5) .
N2 Cd1 2.373(5) .
N97 N98 1.146(8) .
N98 N99 1.167(7) .
N99 Cd1 2.247(5) .
O1 Cd1 2.246(4) 26_565
O1 Cd1 2.392(3) .
O1 Cd1 2.449(4) 3_655
Cd1 O1 2.246(4) 20_656
Cd1 O1 2.449(4) 3_655
