#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:49:32 +0300 (Fri, 06 May 2016) $
#$Revision: 182642 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/44/7224450.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_7224450
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 N20 O8'
_chemical_formula_sum            'C46 H40 Cd4 N20 O8'
_chemical_formula_weight         1450.58
_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                 107.628(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4980(5)
_cell_length_b                   12.6484(6)
_cell_length_c                   15.9441(6)
_cell_measurement_reflns_used    3806
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      27.4800
_cell_measurement_theta_min      3.8500
_cell_volume                     2594.28(19)
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10617
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    1.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85469
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0303
_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)+(0.0301P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                3518
_reflns_number_total             4578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00112b2.cif
_cod_data_source_block           cd79
_cod_depositor_comments
'Adding full bibliography for 7224447--7224455.cif.'
_cod_original_cell_volume        2594.29(19)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7224450
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 0.2453(3) 0.7519(4) 0.4726(3) 0.0515(11) Uani 1 1 d .
H1 H 0.1880 0.7966 0.4561 0.062 Uiso 1 1 calc R
C2 C 0.3431(4) 0.7964(4) 0.4998(3) 0.0662(13) Uani 1 1 d .
H2 H 0.3522 0.8693 0.5016 0.079 Uiso 1 1 calc R
C3 C 0.4254(4) 0.7297(4) 0.5240(4) 0.0797(16) Uani 1 1 d .
H3 H 0.4926 0.7568 0.5422 0.096 Uiso 1 1 calc R
C4 C 0.4104(3) 0.6224(4) 0.5218(3) 0.0653(13) Uani 1 1 d .
H4 H 0.4671 0.5768 0.5383 0.078 Uiso 1 1 calc R
C5 C 0.3109(3) 0.5827(3) 0.4950(2) 0.0428(10) Uani 1 1 d .
C6 C 0.2851(3) 0.4650(3) 0.4934(2) 0.0401(9) Uani 1 1 d .
C7 C 0.2737(3) 0.4146(3) 0.4024(2) 0.0425(10) Uani 1 1 d .
C8 C 0.3283(3) 0.4481(4) 0.3474(3) 0.0640(13) Uani 1 1 d .
H8 H 0.3723 0.5062 0.3625 0.077 Uiso 1 1 calc R
C9 C 0.3172(4) 0.3946(6) 0.2690(3) 0.0852(18) Uani 1 1 d .
H9 H 0.3537 0.4155 0.2308 0.102 Uiso 1 1 calc R
C10 C 0.2501(5) 0.3091(5) 0.2496(3) 0.0842(18) Uani 1 1 d .
H10 H 0.2413 0.2709 0.1980 0.101 Uiso 1 1 calc R
C11 C 0.1971(4) 0.2814(4) 0.3062(3) 0.0662(13) Uani 1 1 d .
H11 H 0.1519 0.2242 0.2922 0.079 Uiso 1 1 calc R
C12 C 0.3905(3) 0.4177(4) 0.6399(3) 0.0676(14) Uani 1 1 d .
H12A H 0.3334 0.3852 0.6541 0.101 Uiso 1 1 calc R
H12B H 0.3946 0.4910 0.6564 0.101 Uiso 1 1 calc R
H12C H 0.4540 0.3828 0.6713 0.101 Uiso 1 1 calc R
C13 C 0.0653(3) 0.5340(4) 0.2313(3) 0.0550(11) Uani 1 1 d .
H13 H 0.1149 0.5875 0.2438 0.066 Uiso 1 1 calc R
C14 C 0.0347(4) 0.4907(4) 0.1478(3) 0.0675(14) Uani 1 1 d .
H14 H 0.0646 0.5127 0.1053 0.081 Uiso 1 1 calc R
C15 C -0.0403(4) 0.4151(4) 0.1295(3) 0.0691(14) Uani 1 1 d .
H15 H -0.0634 0.3855 0.0735 0.083 Uiso 1 1 calc R
C16 C -0.0817(3) 0.3824(4) 0.1935(2) 0.0511(11) Uani 1 1 d .
H16 H -0.1334 0.3309 0.1812 0.061 Uiso 1 1 calc R
C17 C -0.0459(3) 0.4268(3) 0.2769(2) 0.0365(9) Uani 1 1 d .
C18 C -0.0926(2) 0.3977(3) 0.3499(2) 0.0349(9) Uani 1 1 d .
C19 C -0.1191(3) 0.2802(3) 0.3474(2) 0.0379(9) Uani 1 1 d .
C20 C -0.2194(3) 0.2431(4) 0.3133(3) 0.0543(11) Uani 1 1 d .
H20 H -0.2736 0.2899 0.2888 0.065 Uiso 1 1 calc R
C21 C -0.2386(4) 0.1369(4) 0.3159(3) 0.0709(14) Uani 1 1 d .
H21 H -0.3060 0.1110 0.2936 0.085 Uiso 1 1 calc R
C22 C -0.1576(4) 0.0695(4) 0.3518(3) 0.0726(15) Uani 1 1 d .
H22 H -0.1685 -0.0029 0.3537 0.087 Uiso 1 1 calc R
C23 C -0.0604(4) 0.1113(4) 0.3847(3) 0.0626(13) Uani 1 1 d .
H23 H -0.0054 0.0655 0.4093 0.075 Uiso 1 1 calc R
N1 N 0.2290(2) 0.6480(3) 0.46865(19) 0.0405(8) Uani 1 1 d .
N2 N 0.2076(2) 0.3334(3) 0.3816(2) 0.0492(9) Uani 1 1 d .
N3 N 0.0263(2) 0.5019(3) 0.29498(18) 0.0409(8) Uani 1 1 d .
N4 N -0.0399(2) 0.2153(3) 0.3834(2) 0.0475(8) Uani 1 1 d .
N94 N 0.2607(5) 0.0417(5) 0.4299(4) 0.158(3) Uani 1 1 d .
N95 N 0.2282(3) 0.0934(4) 0.4744(3) 0.0782(13) Uani 1 1 d .
N96 N 0.1965(3) 0.1430(3) 0.5215(3) 0.0732(12) Uani 1 1 d .
N97 N -0.0261(4) 0.8438(5) 0.3122(4) 0.122(2) Uani 1 1 d .
N98 N -0.0321(3) 0.7765(3) 0.3573(3) 0.0571(10) Uani 1 1 d .
N99 N -0.0411(3) 0.7079(3) 0.4037(2) 0.0502(9) Uani 1 1 d .
O1 O 0.19872(16) 0.44926(19) 0.51914(15) 0.0355(6) Uani 1 1 d .
O2 O 0.37495(18) 0.4093(2) 0.54787(17) 0.0488(7) Uani 1 1 d .
O3 O -0.02450(16) 0.42079(18) 0.43213(13) 0.0307(5) Uani 1 1 d .
O4 O -0.18448(17) 0.4587(2) 0.33098(15) 0.0437(7) Uani 1 1 d .
H4A H -0.1921 0.4806 0.3770 0.066 Uiso 1 1 calc R
Cd2 Cd 0.111730(19) 0.29311(2) 0.480373(17) 0.03763(10) Uani 1 1 d .
Cd1 Cd 0.069483(18) 0.56844(2) 0.438817(16) 0.03417(9) 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'
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
N1 C1 C2 123.2(4) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C3 C2 C1 117.4(4) . .
C3 C2 H2 121.3 . .
C1 C2 H2 121.3 . .
C2 C3 C4 120.5(4) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C5 119.5(4) . .
C3 C4 H4 120.3 . .
C5 C4 H4 120.3 . .
N1 C5 C4 120.5(4) . .
N1 C5 C6 115.6(3) . .
C4 C5 C6 123.8(4) . .
O1 C6 O2 112.8(3) . .
O1 C6 C5 110.4(3) . .
O2 C6 C5 108.7(3) . .
O1 C6 C7 111.8(3) . .
O2 C6 C7 101.0(3) . .
C5 C6 C7 112.0(3) . .
N2 C7 C8 121.8(4) . .
N2 C7 C6 114.7(3) . .
C8 C7 C6 123.5(4) . .
C7 C8 C9 119.5(5) . .
C7 C8 H8 120.2 . .
C9 C8 H8 120.2 . .
C10 C9 C8 117.8(5) . .
C10 C9 H9 121.1 . .
C8 C9 H9 121.1 . .
C11 C10 C9 119.6(5) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
N2 C11 C10 122.5(5) . .
N2 C11 H11 118.8 . .
C10 C11 H11 118.8 . .
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 122.5(4) . .
N3 C13 H13 118.7 . .
C14 C13 H13 118.7 . .
C15 C14 C13 118.2(4) . .
C15 C14 H14 120.9 . .
C13 C14 H14 120.9 . .
C14 C15 C16 119.9(4) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C17 119.3(4) . .
C15 C16 H16 120.4 . .
C17 C16 H16 120.4 . .
N3 C17 C16 121.2(4) . .
N3 C17 C18 116.9(3) . .
C16 C17 C18 121.8(3) . .
O3 C18 O4 112.0(3) . .
O3 C18 C19 108.3(3) . .
O4 C18 C19 110.0(3) . .
O3 C18 C17 111.2(3) . .
O4 C18 C17 104.1(3) . .
C19 C18 C17 111.2(3) . .
N4 C19 C20 121.6(4) . .
N4 C19 C18 116.0(3) . .
C20 C19 C18 122.3(4) . .
C21 C20 C19 119.5(4) . .
C21 C20 H20 120.2 . .
C19 C20 H20 120.2 . .
C22 C21 C20 119.3(4) . .
C22 C21 H21 120.4 . .
C20 C21 H21 120.4 . .
C23 C22 C21 118.3(5) . .
C23 C22 H22 120.9 . .
C21 C22 H22 120.9 . .
N4 C23 C22 123.4(4) . .
N4 C23 H23 118.3 . .
C22 C23 H23 118.3 . .
C1 N1 C5 118.9(3) . .
C1 N1 Cd1 125.1(3) . .
C5 N1 Cd1 115.4(2) . .
C7 N2 C11 118.7(4) . .
C7 N2 Cd2 117.3(2) . .
C11 N2 Cd2 124.0(3) . .
C17 N3 C13 118.9(3) . .
C17 N3 Cd1 114.7(2) . .
C13 N3 Cd1 126.4(3) . .
C19 N4 C23 117.9(4) . .
C19 N4 Cd2 116.6(2) . .
C23 N4 Cd2 122.4(3) . .
N94 N95 N96 177.7(6) . .
N95 N96 Cd2 122.2(3) . .
N97 N98 N99 178.1(5) . .
N98 N99 Cd1 123.1(3) . .
N98 N99 Cd2 130.8(3) . 3_566
Cd1 N99 Cd2 101.37(13) . 3_566
C6 O1 Cd2 117.4(2) . .
C6 O1 Cd1 107.56(19) . .
Cd2 O1 Cd1 99.79(8) . .
C12 O2 C6 114.8(3) . .
C18 O3 Cd1 115.1(2) . .
C18 O3 Cd1 125.12(19) . 3_566
Cd1 O3 Cd1 101.84(8) . 3_566
C18 O3 Cd2 112.75(19) . .
Cd1 O3 Cd2 100.27(8) . .
Cd1 O3 Cd2 97.85(8) 3_566 .
C18 O4 H4A 109.5 . .
N96 Cd2 O1 118.99(13) . .
N96 Cd2 N99 93.39(14) . 3_566
O1 Cd2 N99 95.21(11) . 3_566
N96 Cd2 N4 95.97(14) . .
O1 Cd2 N4 143.68(10) . .
N99 Cd2 N4 92.01(12) 3_566 .
N96 Cd2 N2 92.54(14) . .
O1 Cd2 N2 69.85(10) . .
N99 Cd2 N2 164.96(13) 3_566 .
N4 Cd2 N2 101.11(11) . .
N96 Cd2 O3 162.38(13) . .
O1 Cd2 O3 77.61(7) . .
N99 Cd2 O3 78.40(9) 3_566 .
N4 Cd2 O3 69.08(9) . .
N2 Cd2 O3 99.31(9) . .
O3 Cd1 N99 108.39(11) . .
O3 Cd1 N1 149.08(10) . .
N99 Cd1 N1 102.49(12) . .
O3 Cd1 O3 78.16(8) . 3_566
N99 Cd1 O3 81.02(10) . 3_566
N1 Cd1 O3 105.78(9) . 3_566
O3 Cd1 N3 71.63(10) . .
N99 Cd1 N3 95.02(11) . .
N1 Cd1 N3 107.48(11) . .
O3 Cd1 N3 146.56(9) 3_566 .
O3 Cd1 O1 78.98(8) . .
N99 Cd1 O1 161.94(10) . .
N1 Cd1 O1 71.05(10) . .
O3 Cd1 O1 84.57(8) 3_566 .
N3 Cd1 O1 102.99(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.331(5) .
C1 C2 1.379(6) .
C1 H1 0.9300 .
C2 C3 1.356(7) .
C2 H2 0.9300 .
C3 C4 1.370(7) .
C3 H3 0.9300 .
C4 C5 1.376(5) .
C4 H4 0.9300 .
C5 N1 1.341(5) .
C5 C6 1.528(5) .
C6 O1 1.363(4) .
C6 O2 1.443(4) .
C6 C7 1.549(5) .
C7 N2 1.335(5) .
C7 C8 1.371(6) .
C8 C9 1.390(7) .
C8 H8 0.9300 .
C9 C10 1.384(7) .
C9 H9 0.9300 .
C10 C11 1.356(7) .
C10 H10 0.9300 .
C11 N2 1.340(5) .
C11 H11 0.9300 .
C12 O2 1.422(5) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 N3 1.341(5) .
C13 C14 1.382(6) .
C13 H13 0.9300 .
C14 C15 1.358(7) .
C14 H14 0.9300 .
C15 C16 1.367(6) .
C15 H15 0.9300 .
C16 C17 1.389(5) .
C16 H16 0.9300 .
C17 N3 1.328(5) .
C17 C18 1.527(5) .
C18 O3 1.385(4) .
C18 O4 1.414(4) .
C18 C19 1.526(5) .
C19 N4 1.331(5) .
C19 C20 1.380(5) .
C20 C21 1.371(6) .
C20 H20 0.9300 .
C21 C22 1.367(7) .
C21 H21 0.9300 .
C22 C23 1.363(6) .
C22 H22 0.9300 .
C23 N4 1.346(5) .
C23 H23 0.9300 .
N1 Cd1 2.291(3) .
N2 Cd2 2.376(3) .
N3 Cd1 2.345(3) .
N4 Cd2 2.373(3) .
N94 N95 1.146(6) .
N95 N96 1.156(5) .
N96 Cd2 2.211(4) .
N97 N98 1.133(5) .
N98 N99 1.170(5) .
N99 Cd1 2.269(3) .
N99 Cd2 2.322(3) 3_566
O1 Cd2 2.285(2) .
O1 Cd1 2.367(2) .
O3 Cd1 2.242(2) .
O3 Cd1 2.319(2) 3_566
O3 Cd2 2.393(2) .
O4 H4A 0.8200 .
Cd2 N99 2.322(3) 3_566
Cd1 O3 2.319(2) 3_566
