#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:59:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180117 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/15/7101591.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_7101591
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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.8880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7707(5)
_cell_length_b                   16.3500(8)
_cell_length_c                   18.0972(9)
_cell_measurement_reflns_used    6711
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.28
_cell_volume                     3139.6(3)
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21988
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.9224
_exptl_absorpt_correction_T_min  0.9224
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         7407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0420
_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)+(0.0487P)²+1.3428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                4824
_reflns_number_total             7407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611654j.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               7101591
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.0000 0.5000 0.0000 0.03185(10) Uani 1 2 d S
S1 S 0.01153(7) 0.44109(5) 0.11757(4) 0.0404(2) Uani 1 1 d .
S2 S 0.21282(7) 0.47242(5) -0.00944(5) 0.03632(19) Uani 1 1 d .
S3 S -0.04876(9) 0.19596(7) 0.14319(6) 0.0616(3) Uani 1 1 d .
O1 O 0.1732(2) 0.19250(12) 0.04743(13) 0.0437(5) Uani 1 1 d .
O2 O 0.0332(3) 0.11898(17) -0.03116(17) 0.0791(9) Uani 1 1 d .
N11 N 0.1896(2) 0.32400(14) 0.10433(14) 0.0335(6) Uani 1 1 d .
N12 N 0.2434(2) 0.40565(15) 0.20137(14) 0.0359(6) Uani 1 1 d .
N21 N 0.1778(2) 0.30738(15) -0.03741(14) 0.0360(6) Uani 1 1 d .
N22 N 0.2703(2) 0.37016(16) -0.12067(14) 0.0397(6) Uani 1 1 d .
N31 N -0.0177(2) 0.28210(15) 0.01943(14) 0.0355(6) Uani 1 1 d .
N32 N -0.2175(2) 0.26646(16) 0.02786(15) 0.0409(6) Uani 1 1 d .
B B 0.1257(3) 0.2759(2) 0.0336(2) 0.0359(8) Uani 1 1 d .
C1 C 0.1176(4) 0.1235(3) 0.0235(3) 0.0659(11) Uani 1 1 d .
C2 C 0.1707(5) 0.0481(3) 0.0663(3) 0.0975(17) Uani 1 1 d .
H2A H 0.1236 0.0003 0.0458 0.146 Uiso 1 1 calc R
H2B H 0.1638 0.0541 0.1188 0.146 Uiso 1 1 calc R
H2C H 0.2586 0.0417 0.0618 0.146 Uiso 1 1 calc R
C11 C 0.1524(3) 0.38935(18) 0.14080(16) 0.0334(7) Uani 1 1 d .
C12 C 0.3069(3) 0.30016(19) 0.14255(17) 0.0378(7) Uani 1 1 d .
H12A H 0.3552 0.2565 0.1290 0.045 Uiso 1 1 calc R
C13 C 0.3402(3) 0.34940(19) 0.20196(18) 0.0398(7) Uani 1 1 d .
H13A H 0.4150 0.3464 0.2373 0.048 Uiso 1 1 calc R
C14 C 0.2435(3) 0.4719(2) 0.25848(18) 0.0419(7) Uani 1 1 d .
C15 C 0.3632(4) 0.4631(2) 0.3175(2) 0.0625(10) Uani 1 1 d .
H15A H 0.3625 0.4106 0.3424 0.094 Uiso 1 1 calc R
H15B H 0.3661 0.5067 0.3542 0.094 Uiso 1 1 calc R
H15C H 0.4367 0.4666 0.2933 0.094 Uiso 1 1 calc R
C16 C 0.2438(4) 0.5545(2) 0.2202(2) 0.0580(10) Uani 1 1 d .
H16A H 0.1673 0.5604 0.1835 0.087 Uiso 1 1 calc R
H16B H 0.3165 0.5583 0.1953 0.087 Uiso 1 1 calc R
H16C H 0.2477 0.5976 0.2574 0.087 Uiso 1 1 calc R
C17 C 0.1294(3) 0.4623(2) 0.29754(19) 0.0541(9) Uani 1 1 d .
H17A H 0.0527 0.4682 0.2610 0.081 Uiso 1 1 calc R
H17B H 0.1320 0.5040 0.3359 0.081 Uiso 1 1 calc R
H17C H 0.1312 0.4086 0.3205 0.081 Uiso 1 1 calc R
C21 C 0.2198(3) 0.38107(18) -0.05685(17) 0.0343(7) Uani 1 1 d .
C22 C 0.1965(3) 0.2515(2) -0.0919(2) 0.0522(9) Uani 1 1 d .
H22A H 0.1731 0.1960 -0.0933 0.063 Uiso 1 1 calc R
C23 C 0.2534(4) 0.2895(2) -0.1423(2) 0.0559(10) Uani 1 1 d .
H23A H 0.2776 0.2655 -0.1848 0.067 Uiso 1 1 calc R
C24 C 0.3345(3) 0.4316(2) -0.16424(19) 0.0465(8) Uani 1 1 d .
C25 C 0.4421(4) 0.4726(3) -0.1117(2) 0.0663(11) Uani 1 1 d .
H25A H 0.4088 0.5019 -0.0728 0.099 Uiso 1 1 calc R
H25B H 0.4848 0.5107 -0.1400 0.099 Uiso 1 1 calc R
H25C H 0.5013 0.4314 -0.0890 0.099 Uiso 1 1 calc R
C26 C 0.3885(4) 0.3859(2) -0.2249(2) 0.0671(11) Uani 1 1 d .
H26A H 0.3206 0.3600 -0.2590 0.101 Uiso 1 1 calc R
H26B H 0.4472 0.3445 -0.2019 0.101 Uiso 1 1 calc R
H26C H 0.4321 0.4242 -0.2524 0.101 Uiso 1 1 calc R
C27 C 0.2389(4) 0.4928(3) -0.2004(3) 0.0829(15) Uani 1 1 d .
H27A H 0.1722 0.4647 -0.2336 0.124 Uiso 1 1 calc R
H27B H 0.2793 0.5318 -0.2290 0.124 Uiso 1 1 calc R
H27C H 0.2035 0.5214 -0.1619 0.124 Uiso 1 1 calc R
C31 C -0.0966(3) 0.24894(19) 0.06277(18) 0.0407(7) Uani 1 1 d .
C32 C -0.0894(3) 0.31995(18) -0.04206(17) 0.0383(7) Uani 1 1 d .
H32A H -0.0579 0.3477 -0.0804 0.046 Uiso 1 1 calc R
C33 C -0.2106(3) 0.31025(19) -0.03735(19) 0.0427(8) Uani 1 1 d .
H33A H -0.2795 0.3296 -0.0720 0.051 Uiso 1 1 calc R
C34 C -0.3364(3) 0.2347(3) 0.0486(2) 0.0596(10) Uani 1 1 d .
C35 C -0.3443(4) 0.2605(4) 0.1289(2) 0.0922(16) Uani 1 1 d .
H35A H -0.3439 0.3197 0.1321 0.138 Uiso 1 1 calc R
H35B H -0.2725 0.2387 0.1629 0.138 Uiso 1 1 calc R
H35C H -0.4215 0.2395 0.1425 0.138 Uiso 1 1 calc R
C36 C -0.3379(4) 0.1419(3) 0.0379(3) 0.0917(16) Uani 1 1 d .
H36A H -0.3327 0.1292 -0.0138 0.138 Uiso 1 1 calc R
H36B H -0.4154 0.1197 0.0501 0.138 Uiso 1 1 calc R
H36C H -0.2664 0.1180 0.0707 0.138 Uiso 1 1 calc R
C37 C -0.4490(3) 0.2724(3) -0.0039(2) 0.0840(15) Uani 1 1 d .
H37A H -0.4462 0.2565 -0.0553 0.126 Uiso 1 1 calc R
H37B H -0.4451 0.3315 0.0002 0.126 Uiso 1 1 calc R
H37C H -0.5268 0.2530 0.0101 0.126 Uiso 1 1 calc R
N1S N -0.3775(4) 0.3157(3) 0.3151(2) 0.1023(15) Uani 1 1 d .
C1S C -0.2733(4) 0.3176(3) 0.3121(2) 0.0717(12) Uani 1 1 d .
C2S C -0.1405(4) 0.3206(3) 0.3080(3) 0.0800(14) Uani 1 1 d .
H2S1 H -0.1265 0.3603 0.2704 0.120 Uiso 1 1 calc R
H2S2 H -0.1128 0.2671 0.2944 0.120 Uiso 1 1 calc R
H2S3 H -0.0932 0.3365 0.3564 0.120 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
S1 Pd S1 180.0 3_565 .
S1 Pd S2 85.01(3) 3_565 .
S1 Pd S2 94.99(3) . .
S1 Pd S2 94.99(3) 3_565 3_565
S1 Pd S2 85.01(3) . 3_565
S2 Pd S2 180.00(4) . 3_565
C11 S1 Pd 109.49(10) . .
C21 S2 Pd 108.95(10) . .
C1 O1 B 128.1(3) . .
C11 N11 C12 107.4(2) . .
C11 N11 B 132.3(2) . .
C12 N11 B 120.2(2) . .
C11 N12 C13 108.2(2) . .
C11 N12 C14 127.6(2) . .
C13 N12 C14 124.2(2) . .
C21 N21 C22 107.8(3) . .
C21 N21 B 133.2(2) . .
C22 N21 B 118.8(3) . .
C21 N22 C23 108.1(3) . .
C21 N22 C24 129.4(3) . .
C23 N22 C24 122.4(3) . .
C31 N31 C32 108.8(2) . .
C31 N31 B 126.1(3) . .
C32 N31 B 125.0(3) . .
C31 N32 C33 108.2(3) . .
C31 N32 C34 126.8(3) . .
C33 N32 C34 124.5(3) . .
O1 B N31 113.9(3) . .
O1 B N11 103.8(2) . .
N31 B N11 113.4(3) . .
O1 B N21 106.3(2) . .
N31 B N21 109.4(2) . .
N11 B N21 109.7(2) . .
O2 C1 O1 123.4(4) . .
O2 C1 C2 121.8(4) . .
O1 C1 C2 114.7(4) . .
N11 C11 N12 108.3(2) . .
N11 C11 S1 126.2(2) . .
N12 C11 S1 125.5(2) . .
C13 C12 N11 109.0(3) . .
C12 C13 N12 107.1(3) . .
N12 C14 C16 109.2(3) . .
N12 C14 C17 109.9(3) . .
C16 C14 C17 111.5(3) . .
N12 C14 C15 108.3(3) . .
C16 C14 C15 109.5(3) . .
C17 C14 C15 108.3(3) . .
N21 C21 N22 107.6(3) . .
N21 C21 S2 126.4(2) . .
N22 C21 S2 126.0(2) . .
C23 C22 N21 108.6(3) . .
C22 C23 N22 107.8(3) . .
C27 C24 N22 109.2(3) . .
C27 C24 C25 111.7(3) . .
N22 C24 C25 109.5(3) . .
C27 C24 C26 109.3(3) . .
N22 C24 C26 108.4(3) . .
C25 C24 C26 108.8(3) . .
N31 C31 N32 106.7(3) . .
N31 C31 S3 124.6(2) . .
N32 C31 S3 128.6(2) . .
C33 C32 N31 108.2(3) . .
C32 C33 N32 108.1(3) . .
N32 C34 C36 107.8(3) . .
N32 C34 C35 109.5(3) . .
C36 C34 C35 113.1(4) . .
N32 C34 C37 109.0(3) . .
C36 C34 C37 109.3(4) . .
C35 C34 C37 108.0(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 S1 2.3193(8) 3_565
Pd S1 2.3193(8) .
Pd S2 2.3710(7) .
Pd S2 2.3710(7) 3_565
S1 C11 1.725(3) .
S2 C21 1.730(3) .
S3 C31 1.696(3) .
O1 C1 1.316(5) .
O1 B 1.463(4) .
O2 C1 1.225(5) .
N11 C11 1.352(4) .
N11 C12 1.388(4) .
N11 B 1.558(4) .
N12 C11 1.366(4) .
N12 C13 1.389(4) .
N12 C14 1.497(4) .
N21 C21 1.355(4) .
N21 C22 1.385(4) .
N21 B 1.575(4) .
N22 C21 1.370(4) .
N22 C23 1.379(4) .
N22 C24 1.515(4) .
N31 C31 1.365(4) .
N31 C32 1.387(4) .
N31 B 1.525(4) .
N32 C31 1.376(4) .
N32 C33 1.393(4) .
N32 C34 1.488(4) .
C1 C2 1.514(6) .
C12 C13 1.342(4) .
C14 C16 1.519(5) .
C14 C17 1.527(5) .
C14 C15 1.534(5) .
C22 C23 1.335(5) .
C24 C27 1.503(5) .
C24 C25 1.523(5) .
C24 C26 1.523(5) .
C32 C33 1.333(4) .
C34 C36 1.528(6) .
C34 C35 1.530(6) .
C34 C37 1.536(5) .
N1S C1S 1.133(5) .
C1S C2S 1.446(6) .
