#------------------------------------------------------------------------------
#$Date: 2018-09-04 17:09:21 +0300 (Tue, 04 Sep 2018) $
#$Revision: 210414 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/35/7113596.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_7113596
loop_
_publ_author_name
'Viton, Florian'
'White, Peter S.'
'Gagné, Michel R.'
_publ_section_title
;
 Crown-ether functionalised second coordination sphere palladium
 catalysts by molecular imprinting
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3040
_journal_page_last               3041
_journal_paper_doi               10.1039/b309072h
_journal_year                    2003
_chemical_formula_moiety         'C32 H26 N2 O7 P2 Pd '
_chemical_formula_sum            'C32 H26 N2 O7 P2 Pd'
_chemical_formula_weight         718.91
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   17.173(3)
_cell_length_b                   17.584(3)
_cell_length_c                   20.164(3)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     6088.9(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Bruker SMART 1K'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            55123
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    0.77
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             2907.28
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       0.31(12)
_refine_ls_extinction_method     Larson
_refine_ls_goodness_of_fit_obs   2.85
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         3951
_refine_ls_R_factor_all          0.077
_refine_ls_R_factor_obs          0.053
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     1/(σ²(F)+0.0000F²)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.056
_refine_ls_wR_factor_obs         0.053
_reflns_number_observed          3967
_reflns_number_total             5389
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_duplicate_entry             7103906
_cod_data_source_file            b309072h.txt
_cod_data_source_block           c03036
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        6088.8(18)
_cod_original_formula_sum        'C32 H26 N2 O7 P2 Pd '
_cod_database_code               7113596
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2-x,1/2+y,z
1/2+x,1/2-y,-z
x,1/2-y,1/2+z
-x,1/2+y,1/2-z
1/2-x,-y,1/2+z
1/2+x,y,1/2-z
loop_
_atom_site_label
_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_type_symbol
Pd1 0.80606(3) 0.04446(3) 0.644992(23) 0.0274(3) Uani Pd
P1 0.68659(10) -0.00438(9) 0.64444(8) 0.0304(9) Uani P
P2 0.78500(10) 0.06265(9) 0.75273(8) 0.0299(9) Uani P
C2 0.6516(4) -0.0142(4) 0.7292(3) 0.035(4) Uani C
C3 0.6814(4) 0.0552(4) 0.7683(3) 0.037(4) Uani C
O4 0.82490(20) 0.03756(22) 0.54435(18) 0.0271(23) Uani O
O5 0.91520(22) 0.09206(20) 0.64334(20) 0.0284(22) Uani O
C11 0.6758(4) -0.0959(4) 0.6054(3) 0.032(4) Uani C
C12 0.7131(4) -0.1092(4) 0.5468(4) 0.050(4) Uani C
C13 0.7079(5) -0.1802(4) 0.5166(4) 0.067(5) Uani C
C14 0.6673(5) -0.2379(4) 0.5469(4) 0.060(5) Uani C
C15 0.6308(5) -0.2251(4) 0.6055(4) 0.060(5) Uani C
C16 0.6354(4) -0.1548(4) 0.6342(3) 0.048(5) Uani C
C21 0.6199(4) 0.0618(4) 0.6053(3) 0.032(4) Uani C
C22 0.5447(4) 0.0401(4) 0.5862(3) 0.048(4) Uani C
C23 0.4955(4) 0.0942(5) 0.5581(4) 0.056(6) Uani C
C24 0.5196(5) 0.1678(5) 0.5507(4) 0.060(5) Uani C
C25 0.5910(5) 0.1899(4) 0.5698(4) 0.060(5) Uani C
C26 0.6419(4) 0.1371(4) 0.5962(4) 0.049(4) Uani C
C31 0.8189(4) 0.1541(4) 0.7826(3) 0.035(4) Uani C
C32 0.7706(5) 0.2089(4) 0.8042(4) 0.062(5) Uani C
C33 0.7987(6) 0.2802(5) 0.8258(4) 0.071(6) Uani C
C34 0.8749(7) 0.2928(5) 0.8243(4) 0.068(6) Uani C
C35 0.9278(5) 0.2381(5) 0.8015(4) 0.068(6) Uani C
C36 0.9000(5) 0.1672(4) 0.7806(4) 0.054(5) Uani C
C41 0.8289(4) -0.0084(4) 0.8069(3) 0.033(4) Uani C
C42 0.8176(4) -0.0052(4) 0.8742(3) 0.045(4) Uani C
C43 0.8477(5) -0.0618(5) 0.9150(4) 0.058(5) Uani C
C44 0.8887(5) -0.1211(5) 0.8872(5) 0.062(5) Uani C
C45 0.9026(5) -0.1237(5) 0.8215(5) 0.067(6) Uani C
C46 0.8717(5) -0.0675(4) 0.7799(4) 0.053(5) Uani C
C51 0.8952(3) 0.0646(3) 0.5306(3) 0.024(3) Uani C
C52 0.9207(4) 0.0641(3) 0.4652(3) 0.027(3) Uani C
C53 0.9955(4) 0.0916(3) 0.4505(3) 0.031(4) Uani C
C54 1.0431(4) 0.1201(3) 0.5001(3) 0.030(4) Uani C
C55 1.0168(3) 0.1222(3) 0.5635(3) 0.029(4) Uani C
C56 0.9424(3) 0.0939(3) 0.5826(3) 0.024(3) Uani C
O57 0.8703(3) 0.03606(23) 0.41832(19) 0.042(3) Uani O
N58 1.0254(4) 0.0887(3) 0.3828(3) 0.050(4) Uani N
O59 0.9870(3) 0.0564(3) 0.33846(24) 0.064(3) Uani O
O60 1.0901(3) 0.1198(3) 0.3729(3) 0.077(4) Uani O
N61 1.0680(4) 0.1544(3) 0.6117(3) 0.041(4) Uani N
O62 1.1387(4) 0.1642(4) 0.5949(3) 0.094(5) Uani O
O63 1.0458(3) 0.1693(3) 0.6658(3) 0.064(4) Uani O
H2a 0.672 -0.060 0.749 0.0451 Uiso H
H2b 0.596 -0.016 0.730 0.0451 Uiso H
H3a 0.655 0.100 0.752 0.0472 Uiso H
H3b 0.672 0.049 0.815 0.0472 Uiso H
H12 0.742 -0.069 0.526 0.0604 Uiso H
H13 0.734 -0.189 0.475 0.0774 Uiso H
H14 0.663 -0.287 0.526 0.0699 Uiso H
H15 0.603 -0.266 0.627 0.0704 Uiso H
H16 0.610 -0.146 0.676 0.0575 Uiso H
H22 0.528 -0.012 0.591 0.0576 Uiso H
H23 0.444 0.080 0.545 0.0661 Uiso H
H24 0.485 0.204 0.531 0.0697 Uiso H
H25 0.607 0.242 0.566 0.0697 Uiso H
H26 0.694 0.152 0.608 0.0592 Uiso H
H32 0.715 0.200 0.804 0.0719 Uiso H
H33 0.764 0.319 0.842 0.0806 Uiso H
H34 0.894 0.341 0.839 0.0782 Uiso H
H35 0.983 0.249 0.800 0.0778 Uiso H
H36 0.935 0.128 0.765 0.0645 Uiso H
H42 0.790 0.037 0.893 0.0547 Uiso H
H43 0.839 -0.059 0.962 0.0682 Uiso H
H44 0.908 -0.161 0.915 0.0718 Uiso H
H45 0.934 -0.164 0.803 0.0769 Uiso H
H46 0.879 -0.070 0.733 0.0627 Uiso H
H54 1.094 0.138 0.490 0.0398 Uiso H
H57 0.833 0.002 0.437 0.0516 Uiso H
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.003 0.002 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
N 0.006 0.003 'International Tables Vol. IV Table 2.2B'
O 0.011 0.006 'International Tables Vol. IV Table 2.2B'
P 0.102 0.094 'International Tables Vol. IV Table 2.2B'
Pd -0.999 1.007 'International Tables Vol. IV Table 2.2B'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P(1) Pd(1) P(2) 84.87(6)
P(1) Pd(1) O(4) 96.74(11)
P(1) Pd(1) O(5) 178.18(12)
P(1) Pd(1) C(51) 123.43(13)
P(1) Pd(1) C(56) 152.87(13)
P(2) Pd(1) O(4) 175.10(12)
P(2) Pd(1) O(5) 96.06(12)
P(2) Pd(1) C(51) 151.35(13)
P(2) Pd(1) C(56) 122.05(13)
O(4) Pd(1) O(5) 82.21(15)
O(4) Pd(1) C(51) 26.70(15)
O(4) Pd(1) C(56) 56.16(16)
O(5) Pd(1) C(51) 55.52(16)
O(5) Pd(1) C(56) 26.06(17)
C(51) Pd(1) C(56) 29.46(17)
Pd(1) P(1) C(2) 109.64(21)
Pd(1) P(1) C(11) 116.24(22)
Pd(1) P(1) C(21) 109.71(21)
C(2) P(1) C(11) 106.9(3)
C(2) P(1) C(21) 105.1(3)
C(11) P(1) C(21) 108.6(3)
Pd(1) P(2) C(3) 108.55(21)
Pd(1) P(2) C(31) 113.55(21)
Pd(1) P(2) C(41) 114.81(22)
C(3) P(2) C(31) 108.8(3)
C(3) P(2) C(41) 104.6(3)
C(31) P(2) C(41) 106.0(3)
P(1) C(2) C(3) 107.2(4)
P(2) C(3) C(2) 107.2(4)
Pd(1) O(4) C(51) 109.1(3)
Pd(1) O(5) C(56) 110.5(3)
P(1) C(11) C(12) 118.9(5)
P(1) C(11) C(16) 122.7(5)
C(12) C(11) C(16) 118.3(6)
C(11) C(12) C(13) 120.2(6)
C(12) C(13) C(14) 120.1(7)
C(13) C(14) C(15) 120.0(7)
C(14) C(15) C(16) 119.4(7)
C(11) C(16) C(15) 122.1(7)
P(1) C(21) C(22) 121.9(5)
P(1) C(21) C(26) 119.8(5)
C(22) C(21) C(26) 118.2(6)
C(21) C(22) C(23) 119.1(7)
C(22) C(23) C(24) 120.5(7)
C(23) C(24) C(25) 121.2(7)
C(24) C(25) C(26) 119.6(7)
C(21) C(26) C(25) 121.3(7)
P(2) C(31) C(32) 123.0(6)
P(2) C(31) C(36) 116.8(5)
C(32) C(31) C(36) 120.1(6)
C(31) C(32) C(33) 121.7(8)
C(32) C(33) C(34) 118.5(8)
C(33) C(34) C(35) 122.2(7)
C(34) C(35) C(36) 119.2(8)
C(31) C(36) C(35) 118.2(7)
P(2) C(41) C(42) 120.4(5)
P(2) C(41) C(46) 119.9(5)
C(42) C(41) C(46) 119.7(6)
C(41) C(42) C(43) 120.2(7)
C(42) C(43) C(44) 119.4(7)
C(43) C(44) C(45) 121.1(7)
C(44) C(45) C(46) 119.8(7)
C(41) C(46) C(45) 119.7(7)
Pd(1) C(51) O(4) 44.16(24)
Pd(1) C(51) C(52) 163.0(4)
Pd(1) C(51) C(56) 75.5(3)
O(4) C(51) C(52) 118.8(5)
O(4) C(51) C(56) 119.6(5)
C(52) C(51) C(56) 121.5(5)
C(51) C(52) C(53) 119.1(6)
C(51) C(52) O(57) 117.3(5)
C(53) C(52) O(57) 123.7(5)
C(52) C(53) C(54) 120.8(6)
C(52) C(53) N(58) 120.5(6)
C(54) C(53) N(58) 118.6(6)
C(53) C(54) C(55) 119.6(6)
C(54) C(55) C(56) 122.9(6)
C(54) C(55) N(61) 116.6(6)
C(56) C(55) N(61) 120.5(6)
Pd(1) C(56) O(5) 43.43(25)
Pd(1) C(56) C(51) 75.0(3)
Pd(1) C(56) C(55) 168.9(4)
O(5) C(56) C(51) 118.5(5)
O(5) C(56) C(55) 125.5(5)
C(51) C(56) C(55) 116.1(5)
C(53) N(58) O(59) 120.0(6)
C(53) N(58) O(60) 116.4(6)
O(59) N(58) O(60) 123.6(6)
C(55) N(61) O(62) 117.4(6)
C(55) N(61) O(63) 121.2(6)
O(62) N(61) O(63) 121.4(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd(1) P(1) 2.2242(17)
Pd(1) P(2) 2.2254(17)
Pd(1) O(4) 2.059(4)
Pd(1) O(5) 2.053(4)
Pd(1) C(51) 2.791(6)
Pd(1) C(56) 2.797(6)
P(1) C(2) 1.820(6)
P(1) C(11) 1.801(6)
P(1) C(21) 1.813(6)
P(2) C(3) 1.811(7)
P(2) C(31) 1.813(6)
P(2) C(41) 1.823(6)
C(2) C(3) 1.540(9)
O(4) C(51) 1.327(7)
O(5) C(56) 1.312(7)
C(11) C(12) 1.365(9)
C(11) C(16) 1.375(9)
C(12) C(13) 1.390(10)
C(13) C(14) 1.374(12)
C(14) C(15) 1.357(13)
C(15) C(16) 1.368(11)
C(21) C(22) 1.400(10)
C(21) C(26) 1.389(10)
C(22) C(23) 1.393(11)
C(23) C(24) 1.367(13)
C(24) C(25) 1.344(13)
C(25) C(26) 1.380(11)
C(31) C(32) 1.343(11)
C(31) C(36) 1.413(11)
C(32) C(33) 1.413(11)
C(33) C(34) 1.327(15)
C(34) C(35) 1.401(15)
C(35) C(36) 1.401(11)
C(41) C(42) 1.370(9)
C(41) C(46) 1.385(10)
C(42) C(43) 1.391(11)
C(43) C(44) 1.377(14)
C(44) C(45) 1.348(13)
C(45) C(46) 1.399(11)
C(51) C(52) 1.389(8)
C(51) C(56) 1.421(8)
C(52) C(53) 1.404(9)
C(52) O(57) 1.373(8)
C(53) C(54) 1.386(9)
C(53) N(58) 1.461(9)
C(54) C(55) 1.356(9)
C(55) C(56) 1.424(8)
C(55) N(61) 1.427(8)
N(58) O(59) 1.247(9)
N(58) O(60) 1.255(9)
N(61) O(62) 1.272(9)
N(61) O(63) 1.185(9)
