#------------------------------------------------------------------------------
#$Date: 2016-05-06 03:49:32 +0300 (Fri, 06 May 2016) $
#$Revision: 182642 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/44/7224452.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_7224452
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         'C50 H40 Cd4 N12 O12'
_chemical_formula_sum            'C50 H40 Cd4 N12 O12'
_chemical_formula_weight         1450.54
_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                 106.524(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4790(9)
_cell_length_b                   12.6998(6)
_cell_length_c                   15.9841(13)
_cell_measurement_reflns_used    3120
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      28.8110
_cell_measurement_theta_min      3.4460
_cell_volume                     2623.2(3)
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11587
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64733
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0561
_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)+(0.0903P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1556
_reflns_number_gt                3393
_reflns_number_total             4626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00112b2.cif
_cod_data_source_block           cd131
_cod_depositor_comments
'Adding full bibliography for 7224447--7224455.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7224452
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 0.2532(6) 0.7515(6) 0.0244(6) 0.052(2) Uani 1 1 d .
H1 H 0.3095 0.7971 0.0393 0.063 Uiso 1 1 calc R
C2 C 0.1549(8) 0.7929(8) -0.0024(7) 0.072(3) Uani 1 1 d .
H2 H 0.1444 0.8654 -0.0050 0.086 Uiso 1 1 calc R
C3 C 0.0719(7) 0.7240(7) -0.0254(8) 0.071(3) Uani 1 1 d .
H3 H 0.0046 0.7498 -0.0435 0.085 Uiso 1 1 calc R
C4 C 0.0893(6) 0.6185(7) -0.0214(7) 0.063(3) Uani 1 1 d .
H4 H 0.0340 0.5717 -0.0364 0.076 Uiso 1 1 calc R
C5 C 0.1900(6) 0.5810(6) 0.0051(5) 0.0417(18) Uani 1 1 d .
C6 C 0.2170(5) 0.4631(6) 0.0097(5) 0.0401(18) Uani 1 1 d .
C7 C 0.2275(6) 0.4165(6) 0.0996(5) 0.0433(19) Uani 1 1 d .
C8 C 0.1691(7) 0.4494(9) 0.1560(6) 0.069(3) Uani 1 1 d .
H8 H 0.1223 0.5048 0.1400 0.083 Uiso 1 1 calc R
C9 C 0.1817(10) 0.3993(12) 0.2340(7) 0.089(4) Uani 1 1 d .
H9 H 0.1453 0.4215 0.2723 0.107 Uiso 1 1 calc R
C10 C 0.2489(11) 0.3159(12) 0.2551(7) 0.096(4) Uani 1 1 d .
H10 H 0.2574 0.2801 0.3074 0.116 Uiso 1 1 calc R
C11 C 0.3042(9) 0.2852(7) 0.1982(6) 0.071(3) Uani 1 1 d .
H11 H 0.3490 0.2281 0.2124 0.085 Uiso 1 1 calc R
C12 C 0.1134(7) 0.4080(8) -0.1338(6) 0.064(3) Uani 1 1 d .
H12A H 0.0521 0.3692 -0.1627 0.096 Uiso 1 1 calc R
H12B H 0.1722 0.3765 -0.1467 0.096 Uiso 1 1 calc R
H12C H 0.1062 0.4795 -0.1540 0.096 Uiso 1 1 calc R
C13 C 0.4313(7) 0.5407(7) 0.2677(6) 0.056(2) Uani 1 1 d .
H13 H 0.3819 0.5939 0.2547 0.068 Uiso 1 1 calc R
C14 C 0.4612(8) 0.4996(9) 0.3500(6) 0.070(3) Uani 1 1 d .
H14 H 0.4308 0.5232 0.3920 0.084 Uiso 1 1 calc R
C15 C 0.5348(9) 0.4246(8) 0.3701(6) 0.071(3) Uani 1 1 d .
H15 H 0.5555 0.3961 0.4259 0.085 Uiso 1 1 calc R
C16 C 0.5789(7) 0.3909(7) 0.3077(5) 0.054(2) Uani 1 1 d .
H16 H 0.6314 0.3408 0.3211 0.064 Uiso 1 1 calc R
C17 C 0.5441(5) 0.4327(5) 0.2231(5) 0.0350(16) Uani 1 1 d .
C18 C 0.5921(5) 0.4020(5) 0.1497(4) 0.0323(16) Uani 1 1 d .
C19 C 0.6216(6) 0.2849(5) 0.1557(5) 0.0390(17) Uani 1 1 d .
C20 C 0.7209(6) 0.2496(6) 0.1899(5) 0.051(2) Uani 1 1 d .
H20 H 0.7744 0.2967 0.2135 0.061 Uiso 1 1 calc R
C21 C 0.7405(7) 0.1421(7) 0.1890(6) 0.061(2) Uani 1 1 d .
H21 H 0.8075 0.1167 0.2118 0.073 Uiso 1 1 calc R
C22 C 0.6613(8) 0.0739(6) 0.1545(6) 0.065(3) Uani 1 1 d .
H22 H 0.6729 0.0017 0.1540 0.078 Uiso 1 1 calc R
C23 C 0.5631(7) 0.1152(6) 0.1202(6) 0.053(2) Uani 1 1 d .
H23 H 0.5088 0.0694 0.0955 0.063 Uiso 1 1 calc R
C96 C 0.2751(9) 0.0852(8) 0.0274(7) 0.074(3) Uani 1 1 d .
C99 C 0.5313(6) 0.7811(7) 0.1400(7) 0.058(2) Uani 1 1 d .
N1 N 0.2702(5) 0.6481(5) 0.0296(4) 0.0416(15) Uani 1 1 d .
N2 N 0.2939(5) 0.3364(5) 0.1236(4) 0.0518(18) Uani 1 1 d .
N3 N 0.4717(5) 0.5059(5) 0.2050(4) 0.0396(14) Uani 1 1 d .
N4 N 0.5427(5) 0.2197(5) 0.1212(5) 0.0492(17) Uani 1 1 d .
N96 N 0.3030(6) 0.1463(6) -0.0126(6) 0.072(2) Uani 1 1 d .
N99 N 0.5347(5) 0.7126(5) 0.0931(5) 0.0478(17) Uani 1 1 d .
O1 O 0.3034(3) 0.4472(4) -0.0159(3) 0.0364(11) Uani 1 1 d .
O2 O 0.1277(4) 0.4060(4) -0.0431(3) 0.0470(13) Uani 1 1 d .
O3 O 0.5245(3) 0.4230(3) 0.0688(3) 0.0274(10) Uani 1 1 d .
O4 O 0.6834(4) 0.4630(4) 0.1681(3) 0.0418(12) Uani 1 1 d .
H4A H 0.6920 0.4847 0.1223 0.063 Uiso 1 1 calc R
O96 O 0.2411(10) 0.0223(10) 0.0641(8) 0.177(6) Uani 1 1 d .
O99 O 0.5296(7) 0.8498(7) 0.1909(7) 0.125(4) Uani 1 1 d .
Cd1 Cd 0.43051(4) 0.57022(4) 0.06020(3) 0.0327(2) Uani 1 1 d .
Cd2 Cd 0.39085(4) 0.29222(4) 0.02249(4) 0.0389(2) 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 122.0(8) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
C1 C2 C3 118.3(9) . .
C1 C2 H2 120.8 . .
C3 C2 H2 120.8 . .
C4 C3 C2 119.7(8) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C3 C4 C5 119.6(8) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N1 C5 C4 120.5(7) . .
N1 C5 C6 116.3(6) . .
C4 C5 C6 123.1(7) . .
O1 C6 O2 113.0(6) . .
O1 C6 C7 111.7(6) . .
O2 C6 C7 101.2(5) . .
O1 C6 C5 110.0(6) . .
O2 C6 C5 108.2(6) . .
C7 C6 C5 112.4(6) . .
N2 C7 C8 119.3(8) . .
N2 C7 C6 116.2(7) . .
C8 C7 C6 124.4(8) . .
C9 C8 C7 119.7(11) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 119.0(11) . .
C8 C9 H9 120.5 . .
C10 C9 H9 120.5 . .
C9 C10 C11 119.9(11) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
N2 C11 C10 120.8(11) . .
N2 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
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 121.4(9) . .
N3 C13 H13 119.3 . .
C14 C13 H13 119.3 . .
C15 C14 C13 119.7(9) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 119.5(9) . .
C14 C15 H15 120.3 . .
C16 C15 H15 120.3 . .
C15 C16 C17 119.3(9) . .
C15 C16 H16 120.4 . .
C17 C16 H16 120.4 . .
N3 C17 C16 120.2(7) . .
N3 C17 C18 117.1(6) . .
C16 C17 C18 122.6(7) . .
O3 C18 O4 113.1(5) . .
O3 C18 C19 109.6(5) . .
O4 C18 C19 108.9(6) . .
O3 C18 C17 110.8(5) . .
O4 C18 C17 103.4(5) . .
C19 C18 C17 110.8(5) . .
N4 C19 C20 122.4(7) . .
N4 C19 C18 114.4(6) . .
C20 C19 C18 123.2(7) . .
C19 C20 C21 118.9(8) . .
C19 C20 H20 120.6 . .
C21 C20 H20 120.6 . .
C22 C21 C20 119.9(8) . .
C22 C21 H21 120.0 . .
C20 C21 H21 120.0 . .
C21 C22 C23 118.0(7) . .
C21 C22 H22 121.0 . .
C23 C22 H22 121.0 . .
N4 C23 C22 122.7(8) . .
N4 C23 H23 118.6 . .
C22 C23 H23 118.6 . .
N96 C96 O96 175.8(13) . .
N99 C99 O99 177.6(12) . .
C1 N1 C5 119.8(7) . .
C1 N1 Cd1 124.9(5) . .
C5 N1 Cd1 114.8(5) . .
C11 N2 C7 121.3(8) . .
C11 N2 Cd2 123.2(7) . .
C7 N2 Cd2 115.5(5) . .
C17 N3 C13 120.0(7) . .
C17 N3 Cd1 114.3(5) . .
C13 N3 Cd1 125.7(5) . .
C19 N4 C23 118.1(7) . .
C19 N4 Cd2 117.8(5) . .
C23 N4 Cd2 120.6(5) . .
C96 N96 Cd2 132.7(8) . .
C99 N99 Cd1 128.0(7) . .
C99 N99 Cd2 129.4(6) . 3_665
Cd1 N99 Cd2 100.0(3) . 3_665
C6 O1 Cd2 117.9(4) . .
C6 O1 Cd1 107.6(4) . .
Cd2 O1 Cd1 100.74(17) . .
C12 O2 C6 116.0(6) . .
C18 O3 Cd1 115.5(4) . .
C18 O3 Cd1 124.9(4) . 3_665
Cd1 O3 Cd1 101.63(16) . 3_665
C18 O3 Cd2 113.0(4) . .
Cd1 O3 Cd2 101.30(17) . .
Cd1 O3 Cd2 96.58(15) 3_665 .
C18 O4 H4A 109.5 . .
O3 Cd1 N99 110.5(2) . .
O3 Cd1 N1 148.53(19) . .
N99 Cd1 N1 101.0(2) . .
O3 Cd1 O3 78.37(16) . 3_665
N99 Cd1 O3 82.8(2) . 3_665
N1 Cd1 O3 105.28(18) . 3_665
O3 Cd1 N3 71.37(18) . .
N99 Cd1 N3 95.2(2) . .
N1 Cd1 N3 107.5(2) . .
O3 Cd1 N3 146.86(18) 3_665 .
O3 Cd1 O1 78.25(15) . .
N99 Cd1 O1 162.5(2) . .
N1 Cd1 O1 71.16(19) . .
O3 Cd1 O1 84.34(15) 3_665 .
N3 Cd1 O1 102.01(19) . .
N96 Cd2 O1 117.5(3) . .
N96 Cd2 N99 95.6(3) . 3_665
O1 Cd2 N99 96.6(2) . 3_665
N96 Cd2 N4 98.2(3) . .
O1 Cd2 N4 142.16(19) . .
N99 Cd2 N4 91.9(2) 3_665 .
N96 Cd2 O3 165.4(3) . .
O1 Cd2 O3 76.83(15) . .
N99 Cd2 O3 79.01(19) 3_665 .
N4 Cd2 O3 68.70(17) . .
N96 Cd2 N2 90.7(3) . .
O1 Cd2 N2 69.1(2) . .
N99 Cd2 N2 165.7(2) 3_665 .
N4 Cd2 N2 100.0(2) . .
O3 Cd2 N2 97.71(18) . .
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(10) .
C1 C2 1.376(12) .
C1 H1 0.9300 .
C2 C3 1.385(14) .
C2 H2 0.9300 .
C3 C4 1.359(12) .
C3 H3 0.9300 .
C4 C5 1.386(11) .
C4 H4 0.9300 .
C5 N1 1.343(9) .
C5 C6 1.538(10) .
C6 O1 1.356(8) .
C6 O2 1.452(8) .
C6 C7 1.523(11) .
C7 N2 1.336(10) .
C7 C8 1.418(12) .
C8 C9 1.366(15) .
C8 H8 0.9300 .
C9 C10 1.372(16) .
C9 H9 0.9300 .
C10 C11 1.384(15) .
C10 H10 0.9300 .
C11 N2 1.331(11) .
C11 H11 0.9300 .
C12 O2 1.408(10) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 N3 1.345(10) .
C13 C14 1.366(13) .
C13 H13 0.9300 .
C14 C15 1.346(14) .
C14 H14 0.9300 .
C15 C16 1.367(13) .
C15 H15 0.9300 .
C16 C17 1.403(11) .
C16 H16 0.9300 .
C17 N3 1.319(9) .
C17 C18 1.543(10) .
C18 O3 1.380(8) .
C18 O4 1.412(8) .
C18 C19 1.535(9) .
C19 N4 1.337(9) .
C19 C20 1.370(10) .
C20 C21 1.392(11) .
C20 H20 0.9300 .
C21 C22 1.363(13) .
C21 H21 0.9300 .
C22 C23 1.384(12) .
C22 H22 0.9300 .
C23 N4 1.356(9) .
C23 H23 0.9300 .
C96 N96 1.135(12) .
C96 O96 1.161(14) .
C99 N99 1.159(11) .
C99 O99 1.197(12) .
N1 Cd1 2.299(6) .
N2 Cd2 2.415(7) .
N3 Cd1 2.366(6) .
N4 Cd2 2.385(6) .
N96 Cd2 2.184(7) .
N99 Cd1 2.258(6) .
N99 Cd2 2.341(7) 3_665
O1 Cd2 2.287(5) .
O1 Cd1 2.381(5) .
O3 Cd1 2.241(4) .
O3 Cd1 2.310(5) 3_665
O3 Cd2 2.408(4) .
O4 H4A 0.8200 .
Cd1 O3 2.310(5) 3_665
Cd2 N99 2.341(7) 3_665
