#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:03:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180001 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/95/7029577.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_7029577
loop_
_publ_author_name
'Suzaki, Yuji'
'Saito, Takashi'
'Ide, Tomohito'
'Osakada, Kohtaro'
_publ_section_title
;
 A rhomboid-shaped organic host molecule with small binding space.
 Unsymmetrical and symmetrical inclusion of halonium ions.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6643
_journal_page_last               6649
_journal_paper_doi               10.1039/c3dt53629g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H14 F6 N2 O4 Pd'
_chemical_formula_sum            'C34 H14 F6 N2 O4 Pd'
_chemical_formula_weight         734.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                73.922(7)
_cell_angle_beta                 89.198(6)
_cell_angle_gamma                78.763(6)
_cell_formula_units_Z            1
_cell_length_a                   7.376(3)
_cell_length_b                   9.605(5)
_cell_length_c                   10.808(5)
_cell_measurement_reflns_used    2203
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.1383
_cell_measurement_theta_min      2.2481
_cell_volume                     721.0(6)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics    'Bruker XShell'
_computing_publication_material  'Bruker XShell'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (George Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3438
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         1.963
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.301
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2493
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0378
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2363
_reflns_number_total             2493
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt53629g2.cif
_cod_data_source_block           Pd(OCOCF3)2(cpeb)
_cod_database_code               7029577
#BEGIN Tags that were not found in dictionaries:
_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   0.867
_shelx_estimated_absorpt_t_max   0.957
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Pd01 Pd 0.0000 0.5000 1.0000 0.01106(16) Uani 1 2 d S U P
O001 O -0.0675(3) 0.6143(3) 0.8147(2) 0.0154(5) Uani 1 1 d . U .
F1 F -0.0994(3) 0.7441(3) 0.5681(2) 0.0336(6) Uani 1 1 d . U .
F3 F -0.3277(3) 0.9017(3) 0.6014(2) 0.0392(7) Uani 1 1 d . U .
O002 O -0.2200(3) 0.8210(3) 0.8590(2) 0.0199(6) Uani 1 1 d . U .
N001 N -0.1272(4) 0.3378(3) 0.9790(3) 0.0115(6) Uani 1 1 d . U .
F2 F -0.0504(4) 0.9309(3) 0.6257(3) 0.0476(7) Uani 1 1 d . U .
C00P C 0.4940(4) 0.4355(4) 0.7245(3) 0.0139(7) Uani 1 1 d . U .
C00R C -0.2799(4) 0.3092(4) 1.0456(3) 0.0142(7) Uani 1 1 d . U .
C00A C -0.1370(5) 0.1358(4) 0.8906(3) 0.0142(7) Uani 1 1 d . U .
H00A H -0.0862 0.0776 0.8356 0.017 Uiso 1 1 calc R U .
C00B C 0.4185(4) 0.5257(4) 0.8055(3) 0.0150(7) Uani 1 1 d . U .
C00C C -0.2923(5) 0.1063(4) 0.9597(4) 0.0162(7) Uani 1 1 d . U .
H00C H -0.3475 0.0267 0.9538 0.019 Uiso 1 1 calc R U .
C00D C -0.1510(4) 0.7471(4) 0.7887(3) 0.0141(7) Uani 1 1 d . U .
C00E C 0.4078(4) 0.3220(4) 0.7102(3) 0.0153(7) Uani 1 1 d . U .
C00F C -0.0569(4) 0.2509(4) 0.9028(3) 0.0137(7) Uani 1 1 d . U .
C00G C 0.3523(4) 0.5976(4) 0.8746(3) 0.0138(7) Uani 1 1 d . U .
C00H C -0.3649(4) 0.1945(4) 1.0368(4) 0.0173(8) Uani 1 1 d . U .
H00H H -0.4721 0.1772 1.0837 0.021 Uiso 1 1 calc R U .
C00I C 0.2428(5) 0.2964(4) 0.7778(3) 0.0153(7) Uani 1 1 d . U .
C00J C 0.4828(5) 0.2343(4) 0.6316(3) 0.0170(7) Uani 1 1 d . U .
H00J H 0.4260 0.1565 0.6233 0.020 Uiso 1 1 calc R U .
C00K C 0.7257(5) 0.3736(4) 0.5788(4) 0.0197(8) Uani 1 1 d . U .
H00K H 0.8338 0.3912 0.5333 0.024 Uiso 1 1 calc R U .
C00L C 0.6410(5) 0.2610(4) 0.5652(4) 0.0200(8) Uani 1 1 d . U .
H00L H 0.6913 0.2022 0.5105 0.024 Uiso 1 1 calc R U .
C00M C 0.1069(4) 0.2807(4) 0.8355(3) 0.0135(7) Uani 1 1 d . U .
C00N C 0.6541(5) 0.4602(4) 0.6578(3) 0.0171(7) Uani 1 1 d . U .
H00N H 0.7134 0.5364 0.6668 0.020 Uiso 1 1 calc R U .
C00O C -0.1567(5) 0.8306(4) 0.6436(4) 0.0233(8) Uani 1 1 d . U .
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'
F F 0.0171 0.0103 '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
O001 Pd01 O001 180.00(14) . 2_567 no
O001 Pd01 N001 89.78(11) . 2_567 no
O001 Pd01 N001 90.22(11) 2_567 2_567 no
O001 Pd01 N001 90.22(11) . . no
O001 Pd01 N001 89.78(11) 2_567 . no
N001 Pd01 N001 180.0 2_567 . no
C00D O001 Pd01 119.2(2) . . no
C00F N001 C00R 118.3(3) . . no
C00F N001 Pd01 120.8(2) . . no
C00R N001 Pd01 120.8(2) . . no
C00N C00P C00E 119.3(3) . . no
C00N C00P C00B 120.1(3) . . no
C00E C00P C00B 120.5(3) . . no
N001 C00R C00H 121.8(3) . . no
N001 C00R C00G 117.5(3) . 2_567 no
C00H C00R C00G 120.7(3) . 2_567 no
C00F C00A C00C 119.4(3) . . no
C00F C00A H00A 120.3 . . no
C00C C00A H00A 120.3 . . no
C00G C00B C00P 178.0(4) . . no
C00H C00C C00A 118.9(3) . . no
C00H C00C H00C 120.6 . . no
C00A C00C H00C 120.6 . . no
O002 C00D O001 130.8(3) . . no
O002 C00D C00O 115.6(3) . . no
O001 C00D C00O 113.6(3) . . no
C00J C00E C00P 120.1(3) . . no
C00J C00E C00I 120.1(3) . . no
C00P C00E C00I 119.7(3) . . no
N001 C00F C00A 122.0(3) . . no
N001 C00F C00M 117.6(3) . . no
C00A C00F C00M 120.5(3) . . no
C00B C00G C00R 176.4(4) . 2_567 no
C00C C00H C00R 119.6(3) . . no
C00C C00H H00H 120.2 . . no
C00R C00H H00H 120.2 . . no
C00M C00I C00E 177.0(4) . . no
C00L C00J C00E 119.8(3) . . no
C00L C00J H00J 120.1 . . no
C00E C00J H00J 120.1 . . no
C00N C00K C00L 120.7(3) . . no
C00N C00K H00K 119.6 . . no
C00L C00K H00K 119.6 . . no
C00J C00L C00K 120.0(3) . . no
C00J C00L H00L 120.0 . . no
C00K C00L H00L 120.0 . . no
C00I C00M C00F 175.4(4) . . no
C00K C00N C00P 119.9(3) . . no
C00K C00N H00N 120.0 . . no
C00P C00N H00N 120.0 . . no
F1 C00O F2 107.9(3) . . no
F1 C00O F3 106.6(3) . . no
F2 C00O F3 107.6(3) . . no
F1 C00O C00D 114.1(3) . . no
F2 C00O C00D 109.3(3) . . no
F3 C00O C00D 111.2(3) . . no
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
Pd01 O001 2.015(3) . no
Pd01 O001 2.015(3) 2_567 no
Pd01 N001 2.032(3) 2_567 no
Pd01 N001 2.032(3) . no
O001 C00D 1.260(4) . no
F1 C00O 1.328(4) . no
F3 C00O 1.331(5) . no
O002 C00D 1.219(4) . no
N001 C00F 1.358(4) . no
N001 C00R 1.361(4) . no
F2 C00O 1.329(5) . no
C00P C00N 1.400(5) . no
C00P C00E 1.408(5) . no
C00P C00B 1.430(5) . no
C00R C00H 1.394(5) . no
C00R C00G 1.435(5) 2_567 no
C00A C00F 1.389(5) . no
C00A C00C 1.391(5) . no
C00A H00A 0.9500 . no
C00B C00G 1.191(5) . no
C00C C00H 1.379(5) . no
C00C H00C 0.9500 . no
C00D C00O 1.548(5) . no
C00E C00J 1.393(5) . no
C00E C00I 1.438(5) . no
C00F C00M 1.437(5) . no
C00G C00R 1.435(5) 2_567 no
C00H H00H 0.9500 . no
C00I C00M 1.186(5) . ?
C00J C00L 1.390(5) . ?
C00J H00J 0.9500 . ?
C00K C00N 1.381(5) . ?
C00K C00L 1.391(5) . ?
C00K H00K 0.9500 . ?
C00L H00L 0.9500 . ?
C00N H00N 0.9500 . ?
