#------------------------------------------------------------------------------
#$Date: 2017-03-04 07:18:03 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193147 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/57/4125773.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_4125773
loop_
_publ_author_name
'Preston, Dan'
'Lewis, James E. M.'
'Crowley, James D.'
_publ_section_title
;
 Multicavity [PdnL4](2n+) Cages with Controlled Segregated Binding of
 Different Guests.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2379
_journal_page_last               2386
_journal_paper_doi               10.1021/jacs.6b11982
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C76 H44 B F4 N12 O2 Pd2'
_chemical_formula_weight         1456.84
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0327(3)
_cell_length_b                   20.7974(5)
_cell_length_c                   27.9988(5)
_cell_measurement_reflns_used    22713
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      76.4660
_cell_measurement_theta_min      3.4470
_cell_volume                     11665.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48531
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.121
_diffrn_reflns_theta_min         3.446
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64814
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.811
_exptl_crystal_description
;
'Sun Jan 18 19:52:12 2015'
;
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.2069
_exptl_crystal_size_mid          0.1798
_exptl_crystal_size_min          0.1255
_platon_squeeze_details
;
solvent molecules and counterions that could not be modelled
;
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3325
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3106
_reflns_number_total             3325
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b11982_si_002.cif
_cod_data_source_block           C1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4125773
_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.
;
_platon_squeeze_void_probe_radius 1.20
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
Pd1 Pd 0.29247(2) 0.0000 0.0000 0.0503(2) Uani 1 4 d S T P
N2 N 0.0000 0.1852(2) 0.13488(13) 0.0615(9) Uani 1 2 d S T P
N1 N 0.29211(10) 0.06845(18) 0.05204(13) 0.0593(7) Uani 1 1 d . . .
C8 C 0.05658(14) 0.21007(16) 0.15170(10) 0.0568(6) Uani 1 1 d . . .
C9 C 0.05936(15) 0.26127(16) 0.18428(10) 0.0568(6) Uani 1 1 d . . .
H9 H 0.1010 0.2776 0.1952 0.068 Uiso 1 1 calc R U .
C10 C 0.0000 0.2872(2) 0.20006(14) 0.0583(9) Uani 1 2 d S T P
H10 H 0.0000 0.3226 0.2215 0.070 Uiso 1 2 calc R U P
C1 C 0.3495(2) 0.0884(3) 0.07053(19) 0.0951(16) Uani 1 1 d . . .
H1 H 0.3903 0.0722 0.0581 0.114 Uiso 1 1 calc R U .
C4 C 0.2325(2) 0.1365(2) 0.10422(15) 0.0743(10) Uani 1 1 d . . .
C2 C 0.3509(2) 0.1315(4) 0.1068(3) 0.140(3) Uani 1 1 d . . .
H2 H 0.3923 0.1442 0.1203 0.168 Uiso 1 1 calc R U .
C5 C 0.23423(16) 0.09232(18) 0.06762(12) 0.0605(7) Uani 1 1 d . . .
H5 H 0.1937 0.0787 0.0532 0.073 Uiso 1 1 calc R U .
C7 C 0.11785(17) 0.1826(2) 0.13390(12) 0.0687(8) Uani 1 1 d . . .
C3 C 0.2918(2) 0.1570(4) 0.1241(3) 0.112(3) Uani 1 1 d . . .
H3 H 0.2920 0.1878 0.1492 0.134 Uiso 1 1 calc R U .
C6 C 0.16967(19) 0.1618(2) 0.12010(13) 0.0741(10) Uani 1 1 d . . .
F1 F 0.44367(18) 0.0000 0.0000 0.0623(9) Uani 1 4 d S TU P
F2 F 0.5000 -0.0609(9) 0.0475(6) 0.197(6) Uani 0.5 2 d S TU P
B1 B 0.5000 0.0000 0.0199(13) 0.126(10) Uani 0.5 4 d S TU P
O1 O 0.1322(4) 0.0000 0.0000 0.117(3) Uani 1 4 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 Pd1 N1 91.3(2) 3 20
N1 Pd1 N1 88.7(2) 3 18
N1 Pd1 N1 179.59(12) 20 18
N1 Pd1 N1 179.59(12) 3 .
N1 Pd1 N1 88.7(2) 20 .
N1 Pd1 N1 91.3(2) 18 .
C8 N2 C8 116.7(4) 19 .
C1 N1 C5 120.6(4) . .
C1 N1 Pd1 119.6(2) . .
C5 N1 Pd1 119.8(2) . .
N2 C8 C9 123.9(3) . .
N2 C8 C7 116.6(3) . .
C9 C8 C7 119.4(3) . .
C10 C9 C8 118.1(3) . .
C9 C10 C9 119.2(4) 19 .
N1 C1 C2 121.1(4) . .
C3 C4 C5 119.1(4) . .
C3 C4 C6 121.1(4) . .
C5 C4 C6 119.8(4) . .
C3 C2 C1 119.9(5) . .
N1 C5 C4 120.9(3) . .
C6 C7 C8 177.5(4) . .
C4 C3 C2 118.4(5) . .
C7 C6 C4 179.1(4) . .
B1 F1 B1 52(3) . 17_655
B1 B1 F1 63.8(14) 17_655 .
B1 B1 F1 63.8(14) 17_655 17_655
F1 B1 F1 128(3) . 17_655
B1 B1 F2 121.4(15) 17_655 .
F1 B1 F2 103.3(4) . .
F1 B1 F2 103.3(4) 17_655 .
B1 B1 F2 121.4(15) 17_655 2_655
F1 B1 F2 103.3(4) . 2_655
F1 B1 F2 103.3(4) 17_655 2_655
F2 B1 F2 117(3) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.037(3) 3
Pd1 N1 2.037(3) 20
Pd1 N1 2.037(3) 18
Pd1 N1 2.037(3) .
N2 C8 1.332(3) 19
N2 C8 1.332(3) .
N1 C1 1.327(5) .
N1 C5 1.335(4) .
C8 C9 1.403(4) .
C8 C7 1.443(4) .
C9 C10 1.379(4) .
C10 C9 1.379(4) 19
C1 C2 1.354(7) .
C4 C3 1.379(7) .
C4 C5 1.376(6) .
C4 C6 1.435(5) .
C2 C3 1.386(6) .
C7 C6 1.189(5) .
F1 B1 1.258(16) .
F1 B1 1.258(16) 17_655
F2 B1 1.49(2) .
B1 B1 1.11(7) 17_655
B1 F1 1.258(16) 17_655
B1 F2 1.49(2) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.018 0.045 -0.021 6288 1937 ' '
