#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:26:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180262 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/48/7114837.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_7114837
loop_
_publ_author_name
'Richtzenhain, Heiko'
'Blake, Alexander J.'
'Bruce, Duncan W.'
'Fallis, Ian A.'
'Li, Wan-Sheung'
'Schröder, Martin'
_publ_section_title
;
 Metal-mediated formation of liquid crystals: synthesis, structural and
 thermal analysis of palladium(ii) complexes of crown thioether
 derivativesElectronic supplementary information (ESI) available: Figs.
 1--3 with full captions, Fig. 4: view of the packing of [Pd(7)][BF4]2.
 Fig. 5: schematic of undulating layers in [Pd(7)][BF4]2. See
 http://www.rsc.org/suppdata/cc/b1/b107027b/
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2580
_journal_paper_doi               10.1039/b107027b
_journal_year                    2001
_chemical_formula_structural     'C28 H36 O6 Pd 2+, 2(BF4) -'
_chemical_formula_sum            'C28 H36 B2 F8 O6 Pd S4'
_chemical_formula_weight         876.83
_chemical_name_common            '[16]aneS4-bisanisate-Pd(II)'
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00(5)
_cell_angle_beta                 107.72(3)
_cell_angle_gamma                90.00(5)
_cell_formula_units_Z            2
_cell_length_a                   12.832(5)
_cell_length_b                   10.224(7)
_cell_length_c                   13.609(7)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      10.0
_cell_volume                     1700.7(16)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  'SHELXL93; PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/theta
_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  0.043
_diffrn_reflns_av_sigmaI/netI    0.075
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3375
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       tablet
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.09
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2205
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.153
_refine_ls_restrained_S_obs      1.229
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         -0.098
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.034P)²+1.044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0922
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          1604
_reflns_number_total             2213
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b107027b.txt
_cod_data_source_block           PD16MB
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_geom_bond_publ_flag' value 'Yes' changed to 'yes'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (2
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (2
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.044P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.034P)^2^+1.044P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114837
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd Pd 1.0000 0.0000 1.0000 0.0181(2) Uani 1 d S .
S1 S 0.89400(13) -0.0650(2) 1.10204(12) 0.0238(4) Uani 1 d . .
C2 C 0.9166(5) -0.2375(7) 1.1293(5) 0.029(2) Uani 1 d . .
H2A H 0.8642(5) -0.2680(7) 1.1626(5) 0.035 Uiso 1 calc R .
H2B H 0.9024(5) -0.2841(7) 1.0645(5) 0.035 Uiso 1 calc R .
C3 C 1.0304(6) -0.2718(7) 1.1970(5) 0.028(2) Uani 1 d . .
H3 H 1.0281(6) -0.3616(7) 1.2214(5) 0.033 Uiso 1 calc R .
C4 C 1.1171(6) -0.2666(7) 1.1435(6) 0.031(2) Uani 1 d . .
H4A H 1.0919(6) -0.3160(7) 1.0798(6) 0.037 Uiso 1 calc R .
H4B H 1.1825(6) -0.3090(7) 1.1869(6) 0.037 Uiso 1 calc R .
S5 S 1.15262(13) -0.1019(2) 1.11354(12) 0.0232(5) Uani 1 d . .
C6 C 1.2361(5) -0.1549(8) 1.0335(5) 0.028(2) Uani 1 d . .
H6A H 1.2836(5) -0.2255(8) 1.0682(5) 0.034 Uiso 1 calc R .
H6B H 1.1885(5) -0.1888(8) 0.9688(5) 0.034 Uiso 1 calc R .
C7 C 1.3057(5) -0.0454(7) 1.0108(5) 0.031(2) Uani 1 d . .
H7A H 1.3311(5) -0.0711(7) 0.9534(5) 0.038 Uiso 1 calc R .
H7B H 1.3695(5) -0.0329(7) 1.0705(5) 0.038 Uiso 1 calc R .
C8 C 1.2442(5) 0.0837(7) 0.9849(5) 0.027(2) Uani 1 d . .
H8A H 1.2840(5) 0.1417(7) 0.9539(5) 0.033 Uiso 1 d R .
H8C H 1.2405(5) 0.1234(7) 1.0477(5) 0.033 Uiso 1 d R .
O31 O 1.0662(4) -0.1890(5) 1.2862(3) 0.0288(12) Uani 1 d . .
C32 C 1.0290(6) -0.2207(8) 1.3669(5) 0.027(2) Uani 1 d . .
O32 O 0.9603(4) -0.3014(5) 1.3611(4) 0.0400(14) Uani 1 d . .
C33 C 1.0840(5) -0.1428(7) 1.4595(5) 0.024(2) Uani 1 d . .
C34 C 1.1748(6) -0.0652(7) 1.4667(5) 0.027(2) Uani 1 d . .
H34 H 1.1983(6) -0.0540(7) 1.4091(5) 0.032 Uiso 1 calc R .
C35 C 1.2308(5) -0.0041(8) 1.5583(5) 0.0245(15) Uani 1 d . .
H35 H 1.2925(5) 0.0460(8) 1.5627(5) 0.029 Uiso 1 calc R .
C36 C 1.1936(5) -0.0186(8) 1.6437(5) 0.029(2) Uani 1 d . .
O36 O 1.2454(4) 0.0353(5) 1.7388(4) 0.0344(14) Uani 1 d . .
C36M C 1.3473(6) 0.0994(8) 1.7507(6) 0.044(2) Uani 1 d . .
H36A H 1.3755(6) 0.1329(8) 1.8196(6) 0.067 Uiso 1 calc R .
H36B H 1.3366(6) 0.1703(8) 1.7023(6) 0.067 Uiso 1 calc R .
H36C H 1.3984(6) 0.0381(8) 1.7380(6) 0.067 Uiso 1 calc R .
C37 C 1.1012(5) -0.0927(7) 1.6363(5) 0.026(2) Uani 1 d . .
H37 H 1.0753(5) -0.1004(7) 1.6929(5) 0.032 Uiso 1 calc R .
C38 C 1.0480(6) -0.1547(7) 1.5461(5) 0.026(2) Uani 1 d . .
H38 H 0.9868(6) -0.2056(7) 1.5423(5) 0.031 Uiso 1 calc R .
B B 0.9229(6) -0.3119(7) 0.8300(5) 0.029(2) Uani 1 d D .
F1 F 0.8385(4) -0.2600(5) 0.8571(4) 0.063(2) Uani 1 d D .
F2 F 0.9299(12) -0.2196(18) 0.7514(12) 0.067(6) Uiso 0.40(2) d PD 1
F3 F 0.9003(8) -0.4282(12) 0.7778(13) 0.031(4) Uiso 0.40(2) d PD 1
F4 F 1.0185(9) -0.3198(19) 0.9074(9) 0.045(5) Uiso 0.40(2) d PD 1
F2' F 0.9205(12) -0.2774(25) 0.7299(11) 0.040(6) Uiso 0.29(2) d PD 2
F3' F 0.8991(13) -0.4443(14) 0.8270(19) 0.051(6) Uiso 0.29(2) d PD 2
F4' F 1.0181(9) -0.2705(19) 0.8953(11) 0.008(4) Uiso 0.29(2) d PD 2
F2" F 0.9081(10) -0.3753(18) 0.7398(10) 0.032(5) Uiso 0.308(11) d PD 3
F3" F 0.9660(16) -0.4145(18) 0.9089(14) 0.094(8) Uiso 0.308(11) d PD 3
F4" F 1.0113(11) -0.2253(15) 0.8504(14) 0.054(6) Uiso 0.308(11) d PD 3
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
_geom_angle_publ_flag
S1 Pd S5 90.15(7) . . yes
S1 Pd S5 89.85(7) . 3_757 yes
S1 Pd S1 180.0 3_757 . ?
S5 Pd S5 180.0 . 3_757 ?
C2 S1 C8 95.4(3) . 3_757 ?
C2 S1 Pd 108.4(2) . . ?
C8 S1 Pd 105.9(2) 3_757 . ?
C3 C2 S1 114.6(5) . . ?
O31 C3 C4 107.2(6) . . ?
O31 C3 C2 112.3(6) . . ?
C4 C3 C2 114.6(6) . . ?
C3 C4 S5 114.4(5) . . ?
C4 S5 C6 95.2(3) . . ?
C4 S5 Pd 110.1(3) . . ?
C6 S5 Pd 105.3(2) . . ?
C7 C6 S5 112.9(5) . . ?
C6 C7 C8 112.9(5) . . ?
C7 C8 S1 113.2(5) . 3_757 ?
C32 O31 C3 116.1(6) . . ?
O32 C32 O31 123.0(7) . . ?
O32 C32 C33 125.6(6) . . ?
O31 C32 C33 111.4(6) . . ?
C34 C33 C38 118.4(7) . . ?
C34 C33 C32 122.8(6) . . ?
C38 C33 C32 118.6(6) . . ?
C35 C34 C33 121.1(6) . . ?
C34 C35 C36 119.2(7) . . ?
O36 C36 C37 116.4(6) . . ?
O36 C36 C35 123.5(6) . . ?
C37 C36 C35 120.1(7) . . ?
C36 O36 C36M 116.9(5) . . ?
C38 C37 C36 120.1(6) . . ?
C37 C38 C33 121.1(7) . . ?
F4' B F1 109.8(7) . . ?
F2" B F1 122.2(7) . . ?
F4 B F1 115.0(7) . . ?
F4 B F3 110.5(9) . . ?
F1 B F3 114.8(7) . . ?
F4' B F3' 118.4(11) . . ?
F1 B F3' 101.8(8) . . ?
F2" B F4" 111.4(10) . . ?
F1 B F4" 111.5(8) . . ?
F4' B F2' 108.2(10) . . ?
F1 B F2' 112.6(9) . . ?
F3' B F2' 106.1(10) . . ?
F4 B F2 111.6(9) . . ?
F1 B F2 100.4(8) . . ?
F3 B F2 103.5(9) . . ?
F2" B F3" 103.7(10) . . ?
F1 B F3" 103.4(8) . . ?
F4" B F3" 101.7(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.317(2) . yes
Pd S5 2.338(2) . yes
Pd S1 2.317(2) 3_757 ?
Pd S5 2.338(2) 3_757 ?
S1 C2 1.807(8) . ?
S1 C8 1.817(7) 3_757 ?
C2 C3 1.512(9) . ?
C3 O31 1.436(8) . ?
C3 C4 1.504(9) . ?
C4 S5 1.823(8) . ?
S5 C6 1.827(6) . ?
C6 C7 1.522(10) . ?
C7 C8 1.524(10) . ?
C8 S1 1.817(6) 3_757 ?
O31 C32 1.363(8) . ?
C32 O32 1.192(8) . ?
C32 C33 1.476(10) . ?
C33 C34 1.388(9) . ?
C33 C38 1.396(9) . ?
C34 C35 1.384(9) . ?
C35 C36 1.392(8) . ?
C36 O36 1.377(8) . ?
C36 C37 1.386(10) . ?
O36 C36M 1.428(8) . ?
C37 C38 1.365(9) . ?
B F4' 1.341(12) . ?
B F2" 1.350(13) . ?
B F4 1.354(11) . ?
B F1 1.354(8) . ?
B F3 1.370(11) . ?
B F3' 1.386(14) . ?
B F4" 1.398(13) . ?
B F2' 1.399(13) . ?
B F2 1.450(12) . ?
B F3" 1.483(15) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 S1 C2 C3 176.0(5) 3_757 . y
S1 C2 C3 O31 47.4(7) . . ?
S1 C2 C3 C4 -75.2(7) . . y
O31 C3 C4 S5 -53.8(7) . . ?
C2 C3 C4 S5 71.6(7) . . y
C3 C4 S5 C6 -170.5(5) . . y
C4 S5 C6 C7 -166.5(5) . . y
S5 C6 C7 C8 -42.3(7) . . y
C6 C7 C8 S1 -43.4(7) . 3_757 y
C4 C3 O31 C32 -152.5(6) . . ?
C2 C3 O31 C32 80.8(7) . . ?
C3 O31 C32 O32 -9.0(10) . . ?
C3 O31 C32 C33 171.1(6) . . ?
O32 C32 C33 C34 169.7(7) . . ?
O31 C32 C33 C34 -10.4(9) . . ?
O32 C32 C33 C38 -5.6(11) . . ?
O31 C32 C33 C38 174.2(6) . . ?
C38 C33 C34 C35 2.0(10) . . ?
C32 C33 C34 C35 -173.4(7) . . ?
C33 C34 C35 C36 -1.5(11) . . ?
C34 C35 C36 O36 178.2(7) . . ?
C34 C35 C36 C37 -0.4(11) . . ?
C37 C36 O36 C36M 173.1(7) . . ?
C35 C36 O36 C36M -5.5(10) . . ?
O36 C36 C37 C38 -176.9(6) . . ?
C35 C36 C37 C38 1.8(11) . . ?
C36 C37 C38 C33 -1.2(11) . . ?
C34 C33 C38 C37 -0.7(10) . . ?
C32 C33 C38 C37 174.9(6) . . ?
