#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:46:50 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195079 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042205.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_7042205
loop_
_publ_author_name
'Marcos, Ismael'
'Domarco, Olaya'
'Peinador, Carlos'
'Fenández, Alberto'
'Fernández, Jesús J'
'Vázquez-García, Digna'
'García, Marcos D'
_publ_section_title
;
 Self-assembly of dinuclear Pd(ii)/Pt(ii) metallacyclic receptors
 incorporating N-heterocyclic carbene complexes as corners.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4182
_journal_page_last               4190
_journal_paper_doi               10.1039/c6dt04476j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C66 H66 F48 N19 O0 P8 Pd2'
_chemical_formula_weight         2497.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3158(13)
_cell_length_b                   33.160(3)
_cell_length_c                   35.500(2)
_cell_measurement_reflns_used    7182
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.386
_cell_measurement_theta_min      4.802
_cell_volume                     22738(3)
_computing_cell_refinement
' SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite.'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_data_reduction
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            73947
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.036
_diffrn_reflns_theta_min         1.147
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.7825
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             9912
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.399
_refine_ls_R_factor_all          0.2314
_refine_ls_R_factor_gt           0.1396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1700P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3672
_refine_ls_wR_factor_ref         0.3967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2754
_reflns_number_total             5423
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04476j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7042204--7042205.cif.'
_cod_database_code               7042205
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.952
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.5678(5) 0.1286(4) 0.2657(3) 0.074(3) Uani 1 1 d . . .
C2 C 0.6139(7) 0.1123(4) 0.3211(4) 0.095(4) Uani 1 1 d . . .
H2 H 0.6172 0.1019 0.3460 0.114 Uiso 1 1 calc R U .
C3 C 0.6580(8) 0.1354(5) 0.3042(4) 0.130(6) Uani 1 1 d . . .
H3 H 0.7035 0.1414 0.3126 0.156 Uiso 1 1 calc R U .
C4 C 0.5000 0.0791(6) 0.3028(5) 0.091(5) Uani 1 2 d S T P
H4A H 0.5000 0.0691 0.3291 0.109 Uiso 1 2 calc R U P
H4B H 0.5000 0.0558 0.2854 0.109 Uiso 1 2 calc R U P
C5 C 0.6513(7) 0.1830(5) 0.2461(4) 0.134(6) Uani 1 1 d . . .
H5A H 0.6949 0.1936 0.2563 0.200 Uiso 1 1 calc R U .
H5B H 0.6592 0.1726 0.2206 0.200 Uiso 1 1 calc R U .
H5C H 0.6169 0.2047 0.2452 0.200 Uiso 1 1 calc R U .
C6 C 0.3817(6) 0.0929(4) 0.1800(4) 0.087(4) Uani 1 1 d . . .
H6 H 0.3852 0.0723 0.1985 0.104 Uiso 1 1 calc R U .
C7 C 0.3372(7) 0.0897(5) 0.1515(4) 0.108(4) Uani 1 1 d . . .
H7 H 0.3112 0.0654 0.1498 0.130 Uiso 1 1 calc R U .
C8 C 0.3257(6) 0.1189(4) 0.1239(3) 0.071(3) Uani 1 1 d . . .
C9 C 0.3681(7) 0.1535(4) 0.1283(3) 0.094(4) Uani 1 1 d . . .
H9 H 0.3631 0.1756 0.1115 0.113 Uiso 1 1 calc R U .
C10 C 0.4139(6) 0.1553(4) 0.1553(3) 0.088(4) Uani 1 1 d . . .
H10 H 0.4434 0.1782 0.1562 0.105 Uiso 1 1 calc R U .
C11 C 0.2616(7) 0.0781(6) 0.0784(4) 0.115(5) Uani 1 1 d . . .
H11 H 0.2840 0.0549 0.0882 0.138 Uiso 1 1 calc R U .
C12 C 0.2740(6) 0.1163(5) 0.0947(3) 0.081(4) Uani 1 1 d . . .
C13 C 0.2433(7) 0.1479(5) 0.0790(3) 0.095(4) Uani 1 1 d . . .
H13 H 0.2523 0.1743 0.0883 0.115 Uiso 1 1 calc R U .
C14 C 0.1976(6) 0.1425(5) 0.0489(4) 0.088(4) Uani 1 1 d . . .
H14 H 0.1733 0.1649 0.0386 0.105 Uiso 1 1 calc R U .
C15 C 0.2161(8) 0.0742(5) 0.0474(4) 0.098(4) Uani 1 1 d . . .
H15 H 0.2067 0.0487 0.0365 0.118 Uiso 1 1 calc R U .
C16 C 0.1408(9) 0.1048(7) 0.0000 0.100(6) Uani 1 2 d S T P
H16A H 0.1125 0.0799 0.0000 0.120 Uiso 1 2 calc R U P
H16B H 0.1093 0.1284 0.0000 0.120 Uiso 1 2 calc R U P
N1 N 0.5611(4) 0.1061(3) 0.2956(3) 0.079(3) Uani 1 1 d . . .
N2 N 0.6259(5) 0.1504(4) 0.2704(3) 0.090(3) Uani 1 1 d . . .
N3 N 0.4222(5) 0.1269(3) 0.1819(2) 0.079(3) Uani 1 1 d . . .
N4 N 0.1886(4) 0.1059(5) 0.0349(3) 0.087(3) Uani 1 1 d . . .
Pd1 Pd 0.5000 0.13038(4) 0.22377(3) 0.0765(6) Uani 1 2 d S T P
F1 F 0.2500 0.2500 0.2033(5) 0.236(8) Uani 1 2 d S T P
F2 F 0.3294(5) 0.2520(3) 0.1618(5) 0.232(7) Uani 1 1 d . . .
F3 F 0.2468(5) 0.2980(3) 0.1602(3) 0.168(4) Uani 1 1 d . . .
F4 F 0.2500 0.2500 0.1188(4) 0.304(15) Uani 1 2 d S T P
P1 P 0.2500 0.2500 0.15858(19) 0.1147(19) Uani 1 2 d S T P
F5 F 0.5580(5) 0.0942(3) 0.4275(4) 0.204(5) Uani 1 1 d . U .
F6 F 0.5584(5) 0.1601(4) 0.4135(4) 0.214(5) Uani 1 1 d . U .
F7 F 0.5000 0.1184(7) 0.3813(3) 0.225(7) Uani 1 2 d S TU P
F8 F 0.5000 0.1444(7) 0.4603(4) 0.271(8) Uani 1 2 d S TU P
P2 P 0.5000 0.1265(2) 0.42185(14) 0.113(2) Uani 1 2 d S TU P
F9 F 0.6984(5) 0.0341(2) 0.3349(4) 0.235(5) Uani 1 1 d D U .
F10 F 0.6085(7) 0.0341(2) 0.3747(3) 0.258(6) Uani 1 1 d D U .
F11 F 0.6023(7) 0.0000 0.3207(4) 0.204(6) Uani 1 2 d DS TU P
F12 F 0.7040(11) 0.0000 0.3892(5) 0.382(13) Uani 1 2 d DS TU P
P3 P 0.6524(4) 0.0000 0.3553(2) 0.131(2) Uani 1 2 d S TU P
F13 F 0.5000 0.0338(3) 0.1606(6) 0.307(14) Uani 1 2 d DS T P
F14 F 0.5000 0.0337(3) 0.2240(5) 0.45(3) Uani 1 2 d DS T P
F15 F 0.4172(5) 0.0000 0.1918(5) 0.241(11) Uani 1 2 d DS T P
P4 P 0.5000 0.0000 0.1932(7) 0.238(7) Uani 1 4 d S T P
F16 F 0.3270(10) 0.2626(13) 0.0000 0.333(13) Uani 1 2 d DS TU P
F17 F 0.2176(12) 0.2722(7) 0.0320(5) 0.377(12) Uani 1 1 d D U .
P5 P 0.2500 0.2500 0.0000 0.256(8) Uani 1 4 d DS TU P
C1S C 0.5000 0.2579(6) 0.1902(5) 0.074(4) Uani 1 2 d S TU P
C2S C 0.5000 0.2953(6) 0.1704(8) 0.182(11) Uani 1 2 d S TU P
H2S1 H 0.4865 0.3171 0.1875 0.273 Uiso 0.5 1 calc R U P
H2S2 H 0.4670 0.2939 0.1494 0.273 Uiso 0.5 1 calc R U P
H2S3 H 0.5465 0.3007 0.1605 0.273 Uiso 0.5 1 calc R U P
N1S N 0.5000 0.2291(5) 0.2067(5) 0.105(5) Uani 1 2 d S TU P
C4S C 0.5747(13) 0.0000 0.0000 0.29(3) Uani 1 4 d DS TU P
C3S C 0.6514(12) 0.0000 0.0000 0.194(16) Uani 1 4 d DS TU P
N2S N 0.7130(11) 0.0000 0.0000 0.144(9) Uani 1 4 d DS TU P
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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 N2 106.8(10) . .
N1 C1 Pd1 124.3(9) . .
N2 C1 Pd1 128.8(9) . .
C3 C2 N1 105.6(12) . .
C2 C3 N2 108.0(11) . .
N1 C4 N1 103.5(13) . 20_655
C7 C6 N3 118.2(13) . .
C6 C7 C8 125.5(13) . .
C7 C8 C9 113.1(11) . .
C7 C8 C12 125.0(12) . .
C9 C8 C12 121.8(11) . .
C10 C9 C8 120.5(12) . .
C9 C10 N3 124.4(12) . .
C12 C11 C15 120.4(14) . .
C13 C12 C11 117.5(13) . .
C13 C12 C8 124.2(14) . .
C11 C12 C8 117.8(13) . .
C12 C13 C14 120.0(14) . .
N4 C14 C13 119.2(12) . .
N4 C15 C11 117.5(13) . .
N4 C16 N4 106.5(12) 18 .
C1 N1 C2 112.1(10) . .
C1 N1 C4 123.7(11) . .
C2 N1 C4 124.0(11) . .
C1 N2 C3 106.0(10) . .
C1 N2 C5 127.1(10) . .
C3 N2 C5 126.9(10) . .
C10 N3 C6 118.2(10) . .
C10 N3 Pd1 122.6(9) . .
C6 N3 Pd1 119.0(8) . .
C15 N4 C14 125.3(12) . .
C15 N4 C16 121.1(14) . .
C14 N4 C16 113.6(14) . .
C1 Pd1 C1 82.6(6) . 20_655
C1 Pd1 N3 93.2(4) . 20_655
C1 Pd1 N3 173.7(5) 20_655 20_655
C1 Pd1 N3 173.7(5) . .
C1 Pd1 N3 93.2(4) 20_655 .
N3 Pd1 N3 90.5(5) 20_655 .
F4 P1 F2 94.2(7) . 14
F4 P1 F2 94.2(7) . .
F2 P1 F2 171.5(13) 14 .
F4 P1 F1 180.0 . .
F2 P1 F1 85.8(7) 14 .
F2 P1 F1 85.8(7) . .
F4 P1 F3 92.1(5) . 14
F2 P1 F3 89.5(6) 14 14
F2 P1 F3 90.2(6) . 14
F1 P1 F3 87.9(5) . 14
F4 P1 F3 92.1(5) . .
F2 P1 F3 90.2(6) 14 .
F2 P1 F3 89.5(6) . .
F1 P1 F3 87.9(5) . .
F3 P1 F3 175.8(9) 14 .
F7 P2 F8 167.0(14) . .
F7 P2 F5 90.1(9) . .
F8 P2 F5 99.0(8) . .
F7 P2 F5 90.0(9) . 20_655
F8 P2 F5 99.0(8) . 20_655
F5 P2 F5 91.5(9) . 20_655
F7 P2 F6 87.0(9) . .
F8 P2 F6 83.8(9) . .
F5 P2 F6 89.8(6) . .
F5 P2 F6 176.7(9) 20_655 .
F7 P2 F6 86.9(9) . 20_655
F8 P2 F6 83.8(9) . 20_655
F5 P2 F6 176.7(9) . 20_655
F5 P2 F6 89.8(6) 20_655 20_655
F6 P2 F6 88.8(9) . 20_655
F12 P3 F11 178.7(11) . .
F12 P3 F10 90.4(7) . 19
F11 P3 F10 90.5(6) . 19
F12 P3 F10 90.4(7) . .
F11 P3 F10 90.5(6) . .
F10 P3 F10 92.0(8) 19 .
F12 P3 F9 89.7(7) . .
F11 P3 F9 89.4(6) . .
F10 P3 F9 178.7(7) 19 .
F10 P3 F9 89.3(4) . .
F12 P3 F9 89.7(7) . 19
F11 P3 F9 89.4(6) . 19
F10 P3 F9 89.3(4) 19 19
F10 P3 F9 178.7(8) . 19
F9 P3 F9 89.4(8) . 19
F14 P4 F14 91.3(16) . 2_655
F14 P4 F15 91.2(7) . 2_655
F14 P4 F15 91.2(7) 2_655 2_655
F14 P4 F15 91.2(7) . .
F14 P4 F15 91.2(7) 2_655 .
F15 P4 F15 177(2) 2_655 .
F14 P4 F13 178.4(15) . 2_655
F14 P4 F13 90.3(5) 2_655 2_655
F15 P4 F13 88.8(8) 2_655 2_655
F15 P4 F13 88.8(8) . 2_655
F14 P4 F13 90.3(5) . .
F14 P4 F13 178.4(15) 2_655 .
F15 P4 F13 88.8(8) 2_655 .
F15 P4 F13 88.8(8) . .
F13 P4 F13 88.1(16) 2_655 .
F17 P5 F17 180.0 . 29
F17 P5 F17 99.2(18) . 18
F17 P5 F17 80.8(18) 29 18
F17 P5 F17 80.8(18) . 14
F17 P5 F17 99.2(18) 29 14
F17 P5 F17 180.0(15) 18 14
F17 P5 F16 105.7(13) . .
F17 P5 F16 74.3(13) 29 .
F17 P5 F16 105.7(13) 18 .
F17 P5 F16 74.3(13) 14 .
F17 P5 F16 74.3(13) . 29
F17 P5 F16 105.7(13) 29 29
F17 P5 F16 74.3(13) 18 29
F17 P5 F16 105.7(13) 14 29
F16 P5 F16 180.0 . 29
N1S C1S C2S 178(2) . .
N2S C3S C4S 180.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.303(13) .
C1 N2 1.345(15) .
C1 Pd1 1.984(11) .
C2 C3 1.292(17) .
C2 N1 1.379(14) .
C3 N2 1.440(16) .
C4 N1 1.504(13) .
C4 N1 1.504(13) 20_655
C5 N2 1.468(15) .
C6 C7 1.331(16) .
C6 N3 1.372(14) .
C7 C8 1.394(17) .
C8 C9 1.421(16) .
C8 C12 1.443(16) .
C9 C10 1.304(15) .
C10 N3 1.344(14) .
C11 C12 1.411(18) .
C11 C15 1.411(17) .
C12 C13 1.328(18) .
C13 C14 1.398(17) .
C14 N4 1.324(16) .
C15 N4 1.258(15) .
C16 N4 1.546(14) 18
C16 N4 1.546(14) .
N3 Pd1 2.118(9) .
Pd1 C1 1.984(11) 20_655
Pd1 N3 2.118(9) 20_655
F1 P1 1.589(18) .
F2 P1 1.540(10) .
F3 P1 1.595(9) .
F4 P1 1.413(15) .
P1 F2 1.540(10) 14
P1 F3 1.595(9) 14
F5 P2 1.563(11) .
F6 P2 1.612(11) .
F7 P2 1.465(14) .
F8 P2 1.489(16) .
P2 F5 1.563(11) 20_655
P2 F6 1.612(11) 20_655
F9 P3 1.609(10) .
F10 P3 1.573(10) .
F11 P3 1.563(13) .
F12 P3 1.562(15) .
P3 F10 1.573(10) 19
P3 F9 1.609(10) 19
F13 P4 1.61(2) .
F14 P4 1.56(2) .
F15 P4 1.601(11) .
P4 F14 1.56(2) 2_655
P4 F15 1.601(11) 2_655
P4 F13 1.61(2) 2_655
F16 P5 1.544(16) .
F17 P5 1.492(14) .
P5 F17 1.492(14) 29
P5 F17 1.492(14) 18
P5 F17 1.492(14) 14
P5 F16 1.544(16) 29
C1S N1S 1.120(19) .
C1S C2S 1.43(3) .
C4S C3S 1.483(19) .
C3S N2S 1.190(18) .
