#------------------------------------------------------------------------------
#$Date: 2017-05-06 00:45:07 +0300 (Sat, 06 May 2017) $
#$Revision: 196331 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/53/1545355.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_1545355
loop_
_publ_author_name
'Sørensen, Mikkel A.'
'Weihe, Høgni'
'Vinum, Morten G.'
'Mortensen, Jesper S.'
'Doerrer, Linda H.'
'Bendix, Jesper'
_publ_section_title
;
 Imposing high-symmetry and tuneable geometry on lanthanide centres with
 chelating Pt and Pd metalloligands
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3566
_journal_paper_doi               10.1039/C7SC00135E
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C16 H24 O8 Pd2 S8 Y, C8 H20 N'
_chemical_formula_sum            'C24 H44 N O8 Pd2 S8 Y'
_chemical_formula_weight         1032.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           124
_space_group_name_Hall           '-P 4 2c'
_space_group_name_H-M_alt        'P 4/m c c'
_symmetry_Int_Tables_number      124
_symmetry_space_group_name_Hall  '-P 4 2c'
_symmetry_space_group_name_H-M   'P 4/m c c'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-09 deposited with the CCDC.
2017-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6638(3)
_cell_length_b                   8.6638(3)
_cell_length_c                   25.8747(9)
_cell_measurement_reflns_used    5802
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.35
_cell_volume                     1942.19(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            16013
_diffrn_reflns_theta_full        28.6926
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0647 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.8482.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.7661
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.4869
_refine_diff_density_min         -0.5876
_refine_diff_density_rms         0.1239
_refine_ls_d_res_high            0.7402
_refine_ls_d_res_low             8.6638
_refine_ls_goodness_of_fit_ref   1.0878
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1296
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0864
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0171P)²+1.8521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                1050
_reflns_number_total             1296
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7sc00135e2.cif
_cod_data_source_block           1Y-Pd-RT
_cod_depositor_comments
'Adding full bibliography for 1545338--1545364.cif.'
_cod_database_code               1545355
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-H4c
 0.96 with sigma of 0.02
 C4-H4a
 0.96 with sigma of 0.02
 C4-H4b
 0.96 with sigma of 0.02
3. Others
 Fixed Sof: S1(0.5) O1(0.5) C3(0.5) S1a(0.5) O1a(0.5) H4c(0.59) H4a(0.48)
 H4b(0.43)
4.a Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x,z
3 y,-x,z
4 x,-y,-z+1/2
5 -x,y,-z+1/2
6 -x,-y,z
7 y,x,-z+1/2
8 -y,-x,-z+1/2
9 -x,-y,-z
10 y,-x,-z
11 -y,x,-z
12 -x,y,z-1/2
13 x,-y,z-1/2
14 x,y,-z
15 -y,-x,z-1/2
16 y,x,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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
Y1 Y 0.5 0.5 0.25 0.01936(12) Uani 1.000000 8 S T P .
Pd1 Pd 0.5 0.5 0.394494(11) 0.02502(9) Uani 1.000000 4 S T P .
S1 S 0.2671(4) 0.6310(3) 0.39367(17) 0.0383(6) Uani 0.500000 1 . . . 1
C1 C 0.2080(2) 0.6284(2) 0.33298(8) 0.0282(5) Uani 1.000000 1 . . . .
C2 C 0.0545(3) 0.7038(3) 0.32212(11) 0.0459(6) Uani 1.000000 1 . . . .
H2a H -0.0041(9) 0.710(2) 0.35354(18) 0.0689(10) Uiso 1.000000 1 GR . . .
H2b H 0.0711(3) 0.8057(9) 0.3087(7) 0.0689(10) Uiso 1.000000 1 GR . . .
H2c H -0.0013(10) 0.6434(12) 0.2972(6) 0.0689(10) Uiso 1.000000 1 GR . . .
N1 N 0.0 1.0 0.5 0.0229(9) Uani 1.000000 8 S T P .
O1 O 0.2735(6) 0.5559(5) 0.2952(2) 0.0334(10) Uani 0.500000 1 . . . 1
C4 C -0.0640(7) 0.7125(5) 0.5 0.0646(13) Uani 1.000000 2 DS T P .
C3 C -0.0311(5) 0.8619(5) 0.46492(15) 0.0287(10) Uani 0.500000 1 . . . .
S1a S 0.2448(4) 0.5808(3) 0.39672(17) 0.0356(6) Uani 0.500000 1 . . . 2
O1a O 0.3011(6) 0.6221(5) 0.2980(2) 0.0325(10) Uani 0.500000 1 . . . 2
H4c H -0.081(7) 0.652(6) 0.5305(14) 0.09(2) Uiso 0.590000 1 D . . .
H4a H -0.172(2) 0.719(7) 0.5 0.090(18) Uiso 0.960000 2 DS T P .
H3 H 0.085(4) 0.867(3) 0.4425(11) 0.061(9) Uiso 1.000000 1 . . . .
H4b H 0.035(4) 0.665(6) 0.5 0.09(2) Uiso 0.860000 2 DS T P .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Pd -0.98845 1.01473 19.33190 15.50170 5.29537 0.60584 0.69866 7.98929 25.20520
76.89860 5.26593017578
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Y -2.99864 3.60419 17.77600 10.29460 5.72629 3.26588 1.40290 12.80060 0.12560
104.35400 1.91212999821
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
O1 Y1 O1 65.6(2) . 4_565
O1 Y1 O1 126.8(2) 7 .
O1 Y1 O1 65.6(2) 8_665 3_565
O1 Y1 O1 84.4(2) 2_655 4_565
O1 Y1 O1 84.4(2) 7 6_665
O1 Y1 O1 75.48(12) 2_655 .
O1 Y1 O1 65.6(2) 6_665 5_655
O1 Y1 O1 126.8(2) 3_565 4_565
O1 Y1 O1 156.0(2) 7 3_565
O1 Y1 O1 75.48(12) 3_565 .
O1 Y1 O1 84.4(2) 8_665 .
O1 Y1 O1 119.9(3) 3_565 2_655
O1 Y1 O1 126.8(2) 8_665 6_665
O1 Y1 O1 119.9(3) 5_655 4_565
O1 Y1 O1 75.48(12) 7 4_565
O1 Y1 O1 156.0(2) 5_655 .
O1 Y1 O1 65.6(2) 7 2_655
O1 Y1 O1 126.8(2) 5_655 2_655
O1 Y1 O1 75.48(12) 7 5_655
O1 Y1 O1 84.4(2) 5_655 3_565
O1 Y1 O1 75.48(12) 8_665 4_565
O1 Y1 O1 156.0(2) 6_665 4_565
O1 Y1 O1 156.0(2) 8_665 2_655
O1 Y1 O1 119.9(3) 6_665 .
O1 Y1 O1 75.48(12) 8_665 5_655
O1 Y1 O1 75.48(12) 6_665 2_655
O1 Y1 O1 75.48(12) 6_665 3_565
O1 Y1 O1 119.9(3) 8_665 7
O1a Y1 O1a 86.9(2) . 4_565
O1a Y1 O1a 86.9(2) 7 2_655
O1a Y1 O1a 74.10(11) 8_665 5_655
O1a Y1 O1a 68.1(2) 2_655 4_565
O1a Y1 O1a 74.10(12) 8_665 4_565
O1a Y1 O1a 74.10(12) 2_655 .
O1a Y1 O1a 74.10(11) 7 4_565
O1a Y1 O1a 157.1(2) 3_565 4_565
O1a Y1 O1a 74.10(12) 7 5_655
O1a Y1 O1a 74.10(11) 3_565 .
O1a Y1 O1a 127.0(2) 8_665 2_655
O1a Y1 O1a 116.9(3) 5_655 4_565
O1a Y1 O1a 116.9(3) 8_665 7
O1a Y1 O1a 127.0(2) 5_655 .
O1a Y1 O1a 157.1(2) 7 .
O1a Y1 O1a 157.1(2) 5_655 2_655
O1a Y1 O1a 127.0(2) 7 3_565
O1a Y1 O1a 68.1(2) 5_655 3_565
O1a Y1 O1a 68.1(2) 7 6_665
O1a Y1 O1a 127.0(2) 6_665 4_565
O1a Y1 O1a 68.1(2) 8_665 .
O1a Y1 O1a 116.9(3) 6_665 .
O1a Y1 O1a 86.9(2) 8_665 3_565
O1a Y1 O1a 74.10(12) 6_665 2_655
O1a Y1 O1a 157.1(2) 8_665 6_665
O1a Y1 O1a 74.10(11) 6_665 3_565
O1a Y1 O1a 86.9(2) 6_665 5_655
O1a Y1 O1a 116.9(3) 3_565 2_655
S1 Pd1 S1 178.9(2) 6_665 .
S1 Pd1 S1 90.0 2_655 6_665
S1 Pd1 S1 90.0 2_655 .
S1 Pd1 S1 90.0 3_565 .
S1 Pd1 S1 90.0 3_565 6_665
S1 Pd1 S1 178.9(2) 2_655 3_565
S1a Pd1 S1a 177.1(2) 6_665 .
S1a Pd1 S1a 90.0 2_655 6_665
S1a Pd1 S1a 90.0 2_655 .
S1a Pd1 S1a 90.0 3_565 .
S1a Pd1 S1a 90.0 3_565 6_665
S1a Pd1 S1a 177.1(2) 2_655 3_565
C1 S1 Pd1 105.8(2) . .
O1 C1 S1 126.1(3) . .
O1a C1 S1a 125.3(3) . .
H2a C2 C1 109.5 . .
H2b C2 C1 109.5 . .
H2b C2 H2a 109.5 . .
H2c C2 C1 109.5 . .
H2c C2 H2a 109.5 . .
H2c C2 H2b 109.5 . .
C3 N1 C3 110.73(17) 9_576 3_465
C3 N1 C3 69.27(16) 10_466 14_556
C3 N1 C3 180.0 10_466 2_665
C3 N1 C3 73.0(3) 14_556 .
C3 N1 C3 69.27(16) 11_666 9_576
C3 N1 C3 110.73(16) 14_556 3_465
C3 N1 C3 110.73(16) 10_466 6_575
C3 N1 C3 73.0(3) 11_666 2_665
C3 N1 C3 110.73(17) 11_666 6_575
C3 N1 C3 110.73(17) 14_556 2_665
C3 N1 C3 69.27(16) . 2_665
C3 N1 C3 180.0 14_556 6_575
C3 N1 C3 69.27(17) 6_575 2_665
C3 N1 C3 107.0(3) 14_556 9_576
C3 N1 C3 107.0(3) 6_575 .
C3 N1 C3 110.73(16) 11_666 .
C3 N1 C3 107.0(3) 3_465 2_665
C3 N1 C3 180.0 11_666 3_465
C3 N1 C3 69.27(16) 3_465 .
C3 N1 C3 69.27(17) 11_666 14_556
C3 N1 C3 69.27(17) 3_465 6_575
C3 N1 C3 110.73(17) 10_466 .
C3 N1 C3 110.73(16) 9_576 2_665
C3 N1 C3 69.27(17) 10_466 9_576
C3 N1 C3 180.0 9_576 .
C3 N1 C3 107.0(3) 10_466 11_666
C3 N1 C3 73.0(3) 9_576 6_575
C3 N1 C3 73.0(3) 10_466 3_465
C1 O1 Y1 148.0(3) . 4_565
C3 C4 C3 68.8(3) 14_556 .
H4c C4 C3 90(4) . 14_556
H4c C4 C3 159(4) . .
H4c C4 C3 90(4) 14_556 .
H4c C4 C3 159(4) 14_556 14_556
H4c C4 H4c 111(7) . 14_556
H4a C4 C3 98(3) . 14_556
H4a C4 C3 98(3) . .
H4a C4 H4c 83(4) . 14_556
H4a C4 H4c 83(4) . .
H4b C4 C3 101(3) . 14_556
H4b C4 C3 101(3) . .
H4b C4 H4c 84(4) . 14_556
H4b C4 H4c 84(4) . .
H4b C4 H4a 158(5) . .
C4 C3 N1 109.1(3) . 3_465
C3 C3 N1 53.49(16) 14_556 3_465
C3 C3 N1 55.36(6) 3_465 3_465
C3 C3 N1 55.36(7) 2_665 3_465
C3 C3 C4 125.5(3) 2_665 .
C3 C3 C4 55.60(16) 14_556 .
C3 C3 C4 125.9(3) 3_465 .
H3 C3 N1 96.6(15) . 3_465
H3 C3 N1 97.0(15) 3_465 3_465
H3 C3 C4 118.0(15) 3_465 .
H3 C3 C4 117.8(15) . .
H3 C3 C3 115.8(15) 3_465 2_665
H3 C3 C3 41.3(15) . 2_665
C1 S1a Pd1 102.93(19) . .
C1 O1a Y1 153.3(3) . 4_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O1 2.335(5) 4_565
Y1 O1 2.335(5) 5_655
Y1 O1 2.335(5) 7
Y1 O1 2.335(5) .
Y1 O1 2.335(5) 6_665
Y1 O1 2.335(5) 2_655
Y1 O1 2.335(5) 3_565
Y1 O1 2.335(5) 8_665
Y1 O1a 2.374(5) 4_565
Y1 O1a 2.374(5) 5_655
Y1 O1a 2.374(5) 8_665
Y1 O1a 2.374(5) .
Y1 O1a 2.374(5) 7
Y1 O1a 2.374(5) 2_655
Y1 O1a 2.374(5) 3_565
Y1 O1a 2.374(5) 6_665
Pd1 S1 2.315(4) .
Pd1 S1 2.315(4) 3_565
Pd1 S1 2.315(4) 6_665
Pd1 S1 2.315(4) 2_655
Pd1 S1a 2.320(4) .
Pd1 S1a 2.320(4) 2_655
Pd1 S1a 2.320(4) 3_565
Pd1 S1a 2.320(4) 6_665
S1 C1 1.652(5) .
C1 C2 1.508(3) .
C1 O1 1.293(5) .
C1 S1a 1.730(5) .
C1 O1a 1.213(5) .
C2 H2a 0.9600 .
C2 H2b 0.9600 .
C2 H2c 0.9600 .
N1 C3 1.526(4) 14_556
N1 C3 1.526(4) 6_575
N1 C3 1.526(4) 3_465
N1 C3 1.526(4) 9_576
N1 C3 1.526(4) 2_665
N1 C3 1.526(4) 11_666
N1 C3 1.526(4) .
N1 C3 1.526(4) 10_466
C4 C3 1.606(5) .
C4 C3 1.606(5) 14_556
C4 H4c 0.960(19) 14_556
C4 H4c 0.960(19) .
C4 H4a 0.935(19) .
C4 H4b 0.951(19) .
C3 C3 1.734(6) 3_465
C3 C3 1.815(8) 14_556
C3 C3 1.734(6) 2_665
C3 H3 1.16(3) .
C3 H3 1.15(3) 3_465
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
C4 H4c 1 0.9600 0.0200 -0.0001
C4 H4a 1 0.9600 0.0200 0.0250
C4 H4b 1 0.9600 0.0200 0.0090
