#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:59:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180117 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/15/7101593.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_7101593
loop_
_publ_author_name
'G. Parkin'
'Keliang Pang.'
'Stephanie M. Quan'
_publ_section_title
;
Palladium complexes with Pd-->B dative bonds: Analysis of the bonding
in the palladaboratrane compound [κ4-B(mimBut)3]Pd(PMe3)
;
_journal_issue                   48
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b611654j
_journal_year                    2006
_chemical_formula_sum            'C50 H78 B2 N14 O4 Pd S6'
_chemical_formula_weight         1259.64
_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                93.8670(10)
_cell_angle_beta                 92.8400(10)
_cell_angle_gamma                106.2340(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8342(4)
_cell_length_b                   11.2770(5)
_cell_length_c                   13.6177(6)
_cell_measurement_reflns_used    5252
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.39
_cell_volume                     1589.73(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      243(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11445
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.9479
_exptl_absorpt_correction_T_min  0.8996
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.6216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                5694
_reflns_number_total             7200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611654j.txt
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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               7101593
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 1.0000 0.0000 0.02902(8) Uani 1 2 d S
S1 S 0.70711(5) 0.96855(5) 0.00512(4) 0.03246(13) Uani 1 1 d .
S2 S 0.50630(6) 1.05986(6) 0.16696(4) 0.03973(15) Uani 1 1 d .
S3 S 0.38906(7) 0.81739(8) 0.35834(5) 0.0558(2) Uani 1 1 d .
O1 O 0.60052(16) 0.70284(15) 0.26014(12) 0.0398(4) Uani 1 1 d .
O2 O 0.4372(2) 0.5292(2) 0.22652(16) 0.0662(6) Uani 1 1 d .
N11 N 0.62875(17) 0.74377(17) 0.08702(14) 0.0327(4) Uani 1 1 d .
N12 N 0.73601(17) 0.73613(17) -0.04519(14) 0.0331(4) Uani 1 1 d .
N21 N 0.65636(16) 0.91415(17) 0.22684(13) 0.0312(4) Uani 1 1 d .
N22 N 0.73386(17) 1.10990(18) 0.28234(14) 0.0334(4) Uani 1 1 d .
N31 N 0.42999(17) 0.76826(19) 0.16636(14) 0.0356(4) Uani 1 1 d .
N32 N 0.22522(18) 0.7429(2) 0.19006(15) 0.0416(5) Uani 1 1 d .
B B 0.5737(2) 0.7826(3) 0.18483(19) 0.0331(6) Uani 1 1 d .
C1 C 0.5208(3) 0.5957(3) 0.2829(2) 0.0502(7) Uani 1 1 d .
C2 C 0.5495(4) 0.5675(3) 0.3860(2) 0.0780(11) Uani 1 1 d .
H2A H 0.5096 0.4803 0.3930 0.117 Uiso 1 1 calc R
H2B H 0.5156 0.6175 0.4322 0.117 Uiso 1 1 calc R
H2C H 0.6421 0.5863 0.3994 0.117 Uiso 1 1 calc R
C11 C 0.69021(19) 0.8124(2) 0.01632(16) 0.0310(5) Uani 1 1 d .
C12 C 0.6315(2) 0.6231(2) 0.06578(19) 0.0423(6) Uani 1 1 d .
H12A H 0.5938 0.5555 0.1018 0.051 Uiso 1 1 calc R
C13 C 0.6967(2) 0.6182(2) -0.01435(19) 0.0417(6) Uani 1 1 d .
H13A H 0.7129 0.5471 -0.0444 0.050 Uiso 1 1 calc R
C14 C 0.8188(2) 0.7679(2) -0.13087(18) 0.0378(5) Uani 1 1 d .
C15 C 0.9380(2) 0.8748(3) -0.0976(2) 0.0502(7) Uani 1 1 d .
H15A H 0.9851 0.8518 -0.0431 0.075 Uiso 1 1 calc R
H15B H 0.9119 0.9475 -0.0765 0.075 Uiso 1 1 calc R
H15C H 0.9928 0.8931 -0.1521 0.075 Uiso 1 1 calc R
C16 C 0.8621(3) 0.6546(3) -0.1645(2) 0.0558(7) Uani 1 1 d .
H16A H 0.9078 0.6308 -0.1096 0.084 Uiso 1 1 calc R
H16B H 0.9189 0.6747 -0.2177 0.084 Uiso 1 1 calc R
H16C H 0.7873 0.5865 -0.1876 0.084 Uiso 1 1 calc R
C17 C 0.7398(3) 0.7986(3) -0.21572(19) 0.0506(7) Uani 1 1 d .
H17A H 0.6655 0.7282 -0.2349 0.076 Uiso 1 1 calc R
H17B H 0.7924 0.8172 -0.2714 0.076 Uiso 1 1 calc R
H17C H 0.7113 0.8700 -0.1951 0.076 Uiso 1 1 calc R
C21 C 0.6352(2) 1.0264(2) 0.22622(16) 0.0318(5) Uani 1 1 d .
C22 C 0.7723(2) 0.9284(2) 0.28132(17) 0.0377(5) Uani 1 1 d .
H22A H 0.8111 0.8651 0.2922 0.045 Uiso 1 1 calc R
C23 C 0.8188(2) 1.0469(2) 0.31535(18) 0.0394(6) Uani 1 1 d .
H23A H 0.8958 1.0818 0.3549 0.047 Uiso 1 1 calc R
C24 C 0.7460(2) 1.2438(2) 0.3108(2) 0.0432(6) Uani 1 1 d .
C25 C 0.8656(3) 1.2976(3) 0.3818(2) 0.0615(8) Uani 1 1 d .
H25A H 0.9414 1.2903 0.3497 0.092 Uiso 1 1 calc R
H25B H 0.8569 1.2523 0.4404 0.092 Uiso 1 1 calc R
H25C H 0.8743 1.3843 0.4003 0.092 Uiso 1 1 calc R
C26 C 0.6280(3) 1.2509(3) 0.3651(2) 0.0601(8) Uani 1 1 d .
H26A H 0.5521 1.2256 0.3194 0.090 Uiso 1 1 calc R
H26B H 0.6400 1.3353 0.3925 0.090 Uiso 1 1 calc R
H26C H 0.6171 1.1961 0.4180 0.090 Uiso 1 1 calc R
C27 C 0.7606(3) 1.3144(3) 0.2183(2) 0.0681(9) Uani 1 1 d .
H27A H 0.6814 1.2863 0.1763 0.102 Uiso 1 1 calc R
H27B H 0.8310 1.2993 0.1829 0.102 Uiso 1 1 calc R
H27C H 0.7788 1.4024 0.2371 0.102 Uiso 1 1 calc R
C31 C 0.3467(2) 0.7754(2) 0.23730(18) 0.0391(5) Uani 1 1 d .
C32 C 0.3594(2) 0.7306(2) 0.07642(18) 0.0396(6) Uani 1 1 d .
H32A H 0.3932 0.7172 0.0158 0.048 Uiso 1 1 calc R
C33 C 0.2352(2) 0.7164(2) 0.09055(19) 0.0447(6) Uani 1 1 d .
H33A H 0.1667 0.6927 0.0416 0.054 Uiso 1 1 calc R
C34 C 0.1006(2) 0.7335(3) 0.2381(2) 0.0499(7) Uani 1 1 d .
C35 C 0.1039(3) 0.8601(3) 0.2863(3) 0.0738(10) Uani 1 1 d .
H35A H 0.1006 0.9158 0.2357 0.111 Uiso 1 1 calc R
H35B H 0.1828 0.8931 0.3283 0.111 Uiso 1 1 calc R
H35C H 0.0303 0.8520 0.3258 0.111 Uiso 1 1 calc R
C36 C -0.0112(3) 0.6923(4) 0.1584(3) 0.0823(11) Uani 1 1 d .
H36A H -0.0160 0.6100 0.1294 0.123 Uiso 1 1 calc R
H36B H 0.0029 0.7500 0.1076 0.123 Uiso 1 1 calc R
H36C H -0.0914 0.6907 0.1878 0.123 Uiso 1 1 calc R
C37 C 0.0825(3) 0.6364(3) 0.3126(3) 0.0692(9) Uani 1 1 d .
H37A H 0.0749 0.5560 0.2786 0.104 Uiso 1 1 calc R
H37B H 0.0049 0.6331 0.3462 0.104 Uiso 1 1 calc R
H37C H 0.1563 0.6581 0.3605 0.104 Uiso 1 1 calc R
N1S N 0.8932(4) 0.8326(5) 0.5206(3) 0.1420(19) Uani 1 1 d .
C1S C 0.8026(3) 0.8600(4) 0.5224(3) 0.0799(11) Uani 1 1 d .
C2S C 0.6860(3) 0.8963(4) 0.5250(3) 0.0844(11) Uani 1 1 d .
H2S1 H 0.7069 0.9861 0.5312 0.127 Uiso 1 1 calc R
H2S2 H 0.6398 0.8637 0.5811 0.127 Uiso 1 1 calc R
H2S3 H 0.6324 0.8638 0.4646 0.127 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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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
S2 Pd S2 180.00(3) 2_675 .
S2 Pd S1 84.290(19) 2_675 .
S2 Pd S1 95.71(2) . .
S2 Pd S1 95.71(2) 2_675 2_675
S2 Pd S1 84.290(19) . 2_675
S1 Pd S1 180.0 . 2_675
C11 S1 Pd 108.53(7) . .
C21 S2 Pd 108.68(8) . .
C1 O1 B 126.5(2) . .
C11 N11 C12 107.70(19) . .
C11 N11 B 131.24(19) . .
C12 N11 B 120.75(19) . .
C11 N12 C13 108.03(19) . .
C11 N12 C14 129.02(19) . .
C13 N12 C14 122.92(19) . .
C21 N21 C22 108.01(19) . .
C21 N21 B 132.04(18) . .
C22 N21 B 119.84(19) . .
C21 N22 C23 107.72(19) . .
C21 N22 C24 127.33(19) . .
C23 N22 C24 124.80(19) . .
C31 N31 C32 108.49(19) . .
C31 N31 B 125.72(19) . .
C32 N31 B 125.3(2) . .
C31 N32 C33 108.62(19) . .
C31 N32 C34 126.2(2) . .
C33 N32 C34 125.1(2) . .
O1 B N31 112.52(19) . .
O1 B N21 102.67(18) . .
N31 B N21 115.0(2) . .
O1 B N11 106.92(19) . .
N31 B N11 109.58(19) . .
N21 B N11 109.68(18) . .
O2 C1 O1 123.8(3) . .
O2 C1 C2 124.0(3) . .
O1 C1 C2 112.1(3) . .
N11 C11 N12 107.64(19) . .
N11 C11 S1 126.41(17) . .
N12 C11 S1 125.95(17) . .
C13 C12 N11 108.7(2) . .
C12 C13 N12 107.9(2) . .
N12 C14 C17 109.39(19) . .
N12 C14 C15 109.52(19) . .
C17 C14 C15 112.1(2) . .
N12 C14 C16 108.4(2) . .
C17 C14 C16 108.7(2) . .
C15 C14 C16 108.6(2) . .
N21 C21 N22 107.91(18) . .
N21 C21 S2 126.51(17) . .
N22 C21 S2 125.57(17) . .
C23 C22 N21 108.3(2) . .
C22 C23 N22 108.1(2) . .
N22 C24 C27 109.1(2) . .
N22 C24 C26 108.3(2) . .
C27 C24 C26 112.9(3) . .
N22 C24 C25 109.0(2) . .
C27 C24 C25 109.3(2) . .
C26 C24 C25 108.1(2) . .
N31 C31 N32 106.5(2) . .
N31 C31 S3 125.39(17) . .
N32 C31 S3 128.09(19) . .
C33 C32 N31 108.4(2) . .
C32 C33 N32 107.9(2) . .
N32 C34 C35 109.2(2) . .
N32 C34 C37 109.2(2) . .
C35 C34 C37 111.8(3) . .
N32 C34 C36 108.7(2) . .
C35 C34 C36 109.2(3) . .
C37 C34 C36 108.7(3) . .
N1S C1S C2S 179.6(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd S2 2.3198(6) 2_675
Pd S2 2.3198(6) .
Pd S1 2.3661(5) .
Pd S1 2.3661(5) 2_675
S1 C11 1.737(2) .
S2 C21 1.723(2) .
S3 C31 1.688(2) .
O1 C1 1.340(3) .
O1 B 1.478(3) .
O2 C1 1.202(3) .
N11 C11 1.358(3) .
N11 C12 1.382(3) .
N11 B 1.571(3) .
N12 C11 1.368(3) .
N12 C13 1.379(3) .
N12 C14 1.508(3) .
N21 C21 1.348(3) .
N21 C22 1.390(3) .
N21 B 1.556(3) .
N22 C21 1.368(3) .
N22 C23 1.386(3) .
N22 C24 1.501(3) .
N31 C31 1.368(3) .
N31 C32 1.386(3) .
N31 B 1.526(3) .
N32 C31 1.377(3) .
N32 C33 1.384(3) .
N32 C34 1.509(3) .
C1 C2 1.496(4) .
C12 C13 1.335(3) .
C14 C17 1.519(3) .
C14 C15 1.524(3) .
C14 C16 1.530(4) .
C22 C23 1.331(3) .
C24 C27 1.526(4) .
C24 C26 1.527(4) .
C24 C25 1.529(4) .
C32 C33 1.335(3) .
C34 C35 1.520(4) .
C34 C37 1.522(4) .
C34 C36 1.533(4) .
N1S C1S 1.109(5) .
C1S C2S 1.434(5) .
