#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:09:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180126 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/24/7102451.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_7102451
loop_
_publ_author_name
'Panda, Snigdha'
'Singh, Harkesh B'
'Butcher, Ray J'
_publ_section_title
;
 Contrasting coordination behaviour of 22-membered chalcogenaaza (Se,
 Te) macrocylces towards Pd(II) and Pt(II): isolation and structural
 characterization of the first metallamacrocyle with a C-Pt-Se linkage.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              322
_journal_page_last               323
_journal_paper_doi               10.1039/b312358h
_journal_year                    2004
_chemical_formula_sum            'C32 H36 F12 N4 P2 Pd Se2'
_chemical_formula_weight         1030.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.622(2)
_cell_angle_beta                 117.296(2)
_cell_angle_gamma                103.042(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9501(14)
_cell_length_b                   10.5010(15)
_cell_length_c                   10.6403(16)
_cell_measurement_temperature    168(2)
_cell_volume                     885.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5787
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    2.765
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.6350
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            'very pale y'
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0009(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0315P)²+0.6220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                3317
_reflns_number_total             4045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312358h.txt
_cod_data_source_block           compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102451
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd Pd 0.5000 0.5000 0.5000 0.01625(10) Uani 1 2 d S
Se Se 0.74026(4) 0.88294(4) 0.96277(4) 0.02432(11) Uani 1 1 d .
P P 0.81953(11) 0.56927(9) 1.20694(10) 0.0233(2) Uani 1 1 d .
F1 F 0.7639(4) 0.4033(3) 1.1621(3) 0.0682(9) Uani 1 1 d .
F2 F 0.6953(3) 0.5705(3) 1.2637(3) 0.0478(6) Uani 1 1 d .
F3 F 0.8754(3) 0.7357(2) 1.2567(3) 0.0556(7) Uani 1 1 d .
F4 F 0.9443(3) 0.5695(3) 1.1531(3) 0.0564(8) Uani 1 1 d .
F5 F 0.6828(3) 0.5466(3) 1.0394(3) 0.0457(6) Uani 1 1 d .
F6 F 0.9600(3) 0.5938(3) 1.3753(3) 0.0479(6) Uani 1 1 d .
N1A N 0.6399(3) 0.5253(3) 0.7264(3) 0.0215(6) Uani 1 1 d .
H1AA H 0.5921 0.5599 0.7767 0.016(9) Uiso 1 1 calc R
N1B N 0.4515(3) 0.6806(3) 0.5447(3) 0.0183(5) Uani 1 1 d .
H1BA H 0.5521 0.7564 0.5973 0.032(11) Uiso 1 1 calc R
C1A C 0.8121(4) 0.8674(3) 0.8211(4) 0.0200(7) Uani 1 1 d .
C2A C 0.8288(4) 0.9752(4) 0.7676(4) 0.0245(7) Uani 1 1 d .
H2AA H 0.8123 1.0575 0.8064 0.018(9) Uiso 1 1 calc R
C3A C 0.8692(4) 0.9633(4) 0.6588(4) 0.0292(8) Uani 1 1 d .
H3AA H 0.8780 1.0361 0.6208 0.042(12) Uiso 1 1 calc R
C4A C 0.8968(4) 0.8450(4) 0.6054(4) 0.0319(8) Uani 1 1 d .
H4AA H 0.9235 0.8359 0.5295 0.026(10) Uiso 1 1 calc R
C5A C 0.8857(4) 0.7394(4) 0.6617(4) 0.0279(8) Uani 1 1 d .
H5AA H 0.9090 0.6604 0.6268 0.040(12) Uiso 1 1 calc R
C6A C 0.8408(4) 0.7473(3) 0.7686(4) 0.0218(7) Uani 1 1 d .
C7A C 0.8173(4) 0.6240(3) 0.8162(4) 0.0246(7) Uani 1 1 d .
H7AA H 0.8822 0.5707 0.7999 0.028(10) Uiso 1 1 calc R
H7AB H 0.8587 0.6604 0.9272 0.023(9) Uiso 1 1 calc R
C8A C 0.6208(4) 0.3773(3) 0.7208(4) 0.0239(7) Uani 1 1 d .
H8AA H 0.7002 0.3814 0.8228 0.033(10) Uiso 1 1 calc R
H8AB H 0.5087 0.3240 0.6927 0.022(9) Uiso 1 1 calc R
C1B C 0.5693(4) 0.9474(3) 0.8586(4) 0.0216(7) Uani 1 1 d .
C2B C 0.5969(4) 1.0884(4) 0.9274(4) 0.0256(7) Uani 1 1 d .
H2BA H 0.6996 1.1503 1.0186 0.024(9) Uiso 1 1 calc R
C3B C 0.4755(4) 1.1392(4) 0.8638(4) 0.0264(8) Uani 1 1 d .
H3BA H 0.4950 1.2360 0.9108 0.023(9) Uiso 1 1 calc R
C4B C 0.3252(5) 1.0485(4) 0.7312(4) 0.0299(8) Uani 1 1 d .
H4BA H 0.2409 1.0826 0.6879 0.048(13) Uiso 1 1 calc R
C5B C 0.2982(4) 0.9074(4) 0.6616(4) 0.0270(8) Uani 1 1 d .
H5BA H 0.1956 0.8462 0.5699 0.039(11) Uiso 1 1 calc R
C6B C 0.4190(4) 0.8546(3) 0.7242(4) 0.0198(7) Uani 1 1 d .
C7B C 0.3847(4) 0.7007(3) 0.6461(4) 0.0206(7) Uani 1 1 d .
H7BA H 0.4342 0.6627 0.7253 0.031(10) Uiso 1 1 calc R
H7BB H 0.2647 0.6458 0.5833 0.021(9) Uiso 1 1 calc R
C8B C 0.3487(4) 0.6953(4) 0.3974(4) 0.0242(7) Uani 1 1 d .
H8BA H 0.3767 0.7972 0.4148 0.029(10) Uiso 1 1 calc R
H8BB H 0.2312 0.6519 0.3601 0.011(8) Uiso 1 1 calc R
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'
F F 0.0171 0.0103 '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'
Se Se -0.0929 2.2259 '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
N1B Pd N1B 180.000(1) . 2_666
N1B Pd N1A 83.73(10) . 2_666
N1B Pd N1A 96.27(10) 2_666 2_666
N1B Pd N1A 96.27(10) . .
N1B Pd N1A 83.73(10) 2_666 .
N1A Pd N1A 180.000(1) 2_666 .
C1B Se C1A 96.78(14) . .
F3 P F1 178.19(17) . .
F3 P F5 90.04(15) . .
F1 P F5 91.25(15) . .
F3 P F4 90.40(16) . .
F1 P F4 90.88(17) . .
F5 P F4 89.43(13) . .
F3 P F6 89.40(15) . .
F1 P F6 89.32(15) . .
F5 P F6 178.87(15) . .
F4 P F6 89.59(14) . .
F3 P F2 89.16(15) . .
F1 P F2 89.54(16) . .
F5 P F2 91.22(13) . .
F4 P F2 179.22(17) . .
F6 P F2 89.76(14) . .
C7A N1A C8A 111.9(2) . .
C7A N1A Pd 116.7(2) . .
C8A N1A Pd 105.12(19) . .
C8B N1B C7B 111.9(2) . .
C8B N1B Pd 109.97(19) . .
C7B N1B Pd 117.22(19) . .
C2A C1A C6A 120.6(3) . .
C2A C1A Se 118.8(2) . .
C6A C1A Se 120.5(2) . .
C3A C2A C1A 120.4(3) . .
C2A C3A C4A 119.6(3) . .
C3A C4A C5A 120.3(3) . .
C4A C5A C6A 121.1(3) . .
C5A C6A C1A 117.9(3) . .
C5A C6A C7A 118.8(3) . .
C1A C6A C7A 123.2(3) . .
N1A C7A C6A 111.7(3) . .
C8B C8A N1A 108.1(3) 2_666 .
C2B C1B C6B 120.7(3) . .
C2B C1B Se 117.4(3) . .
C6B C1B Se 121.8(2) . .
C3B C2B C1B 120.3(3) . .
C2B C3B C4B 119.8(3) . .
C3B C4B C5B 119.8(3) . .
C4B C5B C6B 121.1(3) . .
C5B C6B C1B 118.3(3) . .
C5B C6B C7B 119.6(3) . .
C1B C6B C7B 122.1(3) . .
N1B C7B C6B 112.5(3) . .
N1B C8B C8A 109.4(3) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd N1B 2.063(2) .
Pd N1B 2.063(2) 2_666
Pd N1A 2.066(3) 2_666
Pd N1A 2.066(3) .
Se C1B 1.929(3) .
Se C1A 1.933(3) .
P F3 1.581(2) .
P F1 1.582(3) .
P F5 1.586(2) .
P F4 1.587(3) .
P F6 1.598(2) .
P F2 1.606(2) .
N1A C7A 1.505(4) .
N1A C8A 1.505(4) .
N1B C8B 1.497(4) .
N1B C7B 1.505(4) .
C1A C2A 1.392(5) .
C1A C6A 1.400(4) .
C2A C3A 1.378(5) .
C3A C4A 1.381(5) .
C4A C5A 1.385(5) .
C5A C6A 1.393(5) .
C6A C7A 1.506(5) .
C8A C8B 1.503(5) 2_666
C1B C2B 1.388(5) .
C1B C6B 1.398(5) .
C2B C3B 1.383(5) .
C3B C4B 1.387(5) .
C4B C5B 1.391(5) .
C5B C6B 1.391(4) .
C6B C7B 1.509(4) .
C8B C8A 1.503(5) 2_666
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1A H1AA F5 0.93 2.56 3.102(4) 117.2
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
N1B Pd N1A C7A -82.5(2) . .
N1B Pd N1A C7A 97.5(2) 2_666 .
N1A Pd N1A C7A 120(100) 2_666 .
N1B Pd N1A C8A 152.9(2) . .
N1B Pd N1A C8A -27.1(2) 2_666 .
N1A Pd N1A C8A -4(100) 2_666 .
N1B Pd N1B C8B -77(100) 2_666 .
N1A Pd N1B C8B -0.6(2) 2_666 .
N1A Pd N1B C8B 179.4(2) . .
N1B Pd N1B C7B 52(100) 2_666 .
N1A Pd N1B C7B 128.7(2) 2_666 .
N1A Pd N1B C7B -51.3(2) . .
C1B Se C1A C2A 43.2(3) . .
C1B Se C1A C6A -134.4(3) . .
C6A C1A C2A C3A 1.9(5) . .
Se C1A C2A C3A -175.7(3) . .
C1A C2A C3A C4A -1.5(5) . .
C2A C3A C4A C5A -0.7(5) . .
C3A C4A C5A C6A 2.4(5) . .
C4A C5A C6A C1A -1.9(5) . .
C4A C5A C6A C7A 175.1(3) . .
C2A C1A C6A C5A -0.2(5) . .
Se C1A C6A C5A 177.4(2) . .
C2A C1A C6A C7A -177.1(3) . .
Se C1A C6A C7A 0.5(4) . .
C8A N1A C7A C6A 155.7(3) . .
Pd N1A C7A C6A 34.6(3) . .
C5A C6A C7A N1A -96.5(4) . .
C1A C6A C7A N1A 80.4(4) . .
C7A N1A C8A C8B -78.3(3) . 2_666
Pd N1A C8A C8B 49.2(3) . 2_666
C1A Se C1B C2B -108.0(3) . .
C1A Se C1B C6B 76.1(3) . .
C6B C1B C2B C3B 0.0(5) . .
Se C1B C2B C3B -176.0(3) . .
C1B C2B C3B C4B 0.4(5) . .
C2B C3B C4B C5B -0.9(6) . .
C3B C4B C5B C6B 1.0(6) . .
C4B C5B C6B C1B -0.5(5) . .
C4B C5B C6B C7B 179.6(3) . .
C2B C1B C6B C5B 0.0(5) . .
Se C1B C6B C5B 175.9(3) . .
C2B C1B C6B C7B 179.9(3) . .
Se C1B C6B C7B -4.2(4) . .
C8B N1B C7B C6B -75.6(3) . .
Pd N1B C7B C6B 156.1(2) . .
C5B C6B C7B N1B 97.7(4) . .
C1B C6B C7B N1B -82.2(4) . .
C7B N1B C8B C8A -158.8(3) . 2_666
Pd N1B C8B C8A -26.7(3) . 2_666
