#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:50:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179818 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/14/7011451.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_7011451
loop_
_publ_author_name
'Rheingold, Arnold L.'
'Liable-Sands, Louise M.'
'Incarvito, Christopher L.'
'Trofimenko, Swiatoslaw'
_publ_section_title
;
 Novel scorpionate ligands devoid of C--H bonds: BpBr3 and TpBr3
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2297
_journal_paper_doi               10.1039/b111568p
_journal_year                    2002
_chemical_formula_sum            'C13 H8 B Br9 N6 Pd'
_chemical_formula_weight         1084.65
_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                101.967(2)
_cell_angle_beta                 92.483(2)
_cell_angle_gamma                104.979(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1589(3)
_cell_length_b                   10.4504(3)
_cell_length_c                   12.6714(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1264.60(6)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12592
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    14.967
_exptl_absorpt_correction_T_max  0.3160
_exptl_absorpt_correction_T_min  0.1176
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0437P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                4569
_reflns_number_total             5946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111568p.txt
_cod_data_source_block           5
_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               7011451
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.27715(4) 0.71994(4) 0.33932(3) 0.02062(10) Uani 1 1 d . . .
B1 B 0.1901(6) 0.9219(6) 0.1997(4) 0.0182(12) Uani 1 1 d . . .
H1 H 0.156(5) 0.995(5) 0.160(4) 0.009(12) Uiso 1 1 d . . .
Br1 Br -0.05087(6) 0.80133(6) -0.01711(5) 0.02777(14) Uani 1 1 d . . .
Br2 Br -0.22589(6) 0.46248(6) 0.01885(5) 0.03085(14) Uani 1 1 d . . .
Br3 Br -0.05884(6) 0.43995(6) 0.27151(5) 0.03198(15) Uani 1 1 d . . .
Br4 Br 0.05970(7) 1.17648(7) 0.31833(6) 0.03959(17) Uani 1 1 d . . .
Br5 Br 0.14078(8) 1.20765(7) 0.60608(5) 0.04043(17) Uani 1 1 d . . .
Br6 Br 0.31813(8) 0.94708(7) 0.61696(5) 0.04348(18) Uani 1 1 d . . .
Br7 Br 0.42754(7) 1.20406(6) 0.18570(6) 0.03930(17) Uani 1 1 d . . .
Br8 Br 0.72089(6) 1.07685(7) 0.10509(5) 0.03449(16) Uani 1 1 d . . .
Br9 Br 0.59923(7) 0.70828(7) 0.09929(6) 0.03635(16) Uani 1 1 d . . .
N1 N 0.0940(4) 0.7767(4) 0.1699(3) 0.0164(9) Uani 1 1 d . . .
N2 N 0.0949(4) 0.6875(4) 0.2364(3) 0.0178(9) Uani 1 1 d . . .
N3 N 0.1961(4) 0.9753(4) 0.3250(3) 0.0178(9) Uani 1 1 d . . .
N4 N 0.2569(5) 0.9194(4) 0.3951(4) 0.0202(9) Uani 1 1 d . . .
N5 N 0.3352(5) 0.9212(4) 0.1711(3) 0.0183(9) Uani 1 1 d . . .
N6 N 0.3752(5) 0.8039(5) 0.1507(4) 0.0220(10) Uani 1 1 d . . .
C1 C -0.0119(5) 0.7179(5) 0.0922(4) 0.0201(11) Uani 1 1 d . . .
C2 C -0.0813(5) 0.5924(5) 0.1070(4) 0.0218(11) Uani 1 1 d . . .
C3 C -0.0111(6) 0.5802(5) 0.1989(4) 0.0213(11) Uani 1 1 d . . .
C4 C 0.1511(5) 1.0764(5) 0.3819(4) 0.0208(11) Uani 1 1 d . . .
C5 C 0.1822(6) 1.0871(6) 0.4909(5) 0.0242(12) Uani 1 1 d . . .
C6 C 0.2465(6) 0.9869(5) 0.4938(4) 0.0239(12) Uani 1 1 d . . .
C7 C 0.4395(6) 1.0265(6) 0.1608(4) 0.0222(11) Uani 1 1 d . . .
C8 C 0.5505(6) 0.9781(6) 0.1318(4) 0.0238(12) Uani 1 1 d . . .
C9 C 0.5039(6) 0.8406(6) 0.1283(4) 0.0242(12) Uani 1 1 d . . .
C10 C 0.4622(6) 0.7200(7) 0.4205(6) 0.0360(15) Uani 1 1 d . . .
H10A H 0.5426 0.7297 0.3784 0.043 Uiso 1 1 calc R . .
H10B H 0.4838 0.7733 0.4964 0.043 Uiso 1 1 calc R . .
C11 C 0.3724(6) 0.5884(6) 0.4039(5) 0.0314(14) Uani 1 1 d . . .
C12 C 0.3200(7) 0.5303(6) 0.2952(6) 0.0341(15) Uani 1 1 d . . .
H12A H 0.2404 0.4488 0.2820 0.041 Uiso 1 1 calc R . .
H12B H 0.3882 0.5235 0.2423 0.041 Uiso 1 1 calc R . .
C13 C 0.3130(8) 0.5295(8) 0.4950(7) 0.050(2) Uani 1 1 d . . .
H13A H 0.3672 0.4718 0.5156 0.075 Uiso 1 1 calc R . .
H13B H 0.2182 0.4749 0.4717 0.075 Uiso 1 1 calc R . .
H13C H 0.3144 0.6033 0.5575 0.075 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'
Br Br -0.2901 2.4595 '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
C10 Pd1 C12 68.1(3) . . ?
C10 Pd1 N4 105.1(2) . . ?
C12 Pd1 N4 173.2(2) . . ?
C10 Pd1 N2 169.2(2) . . ?
C12 Pd1 N2 101.7(2) . . ?
N4 Pd1 N2 85.04(17) . . ?
C10 Pd1 C11 38.7(2) . . ?
C12 Pd1 C11 38.6(3) . . ?
N4 Pd1 C11 135.7(2) . . ?
N2 Pd1 C11 133.9(2) . . ?
N5 B1 N1 110.4(4) . . ?
N5 B1 N3 108.4(4) . . ?
N1 B1 N3 107.7(4) . . ?
C1 N1 N2 107.7(4) . . ?
C1 N1 B1 131.0(4) . . ?
N2 N1 B1 120.7(4) . . ?
C3 N2 N1 106.5(4) . . ?
C3 N2 Pd1 133.2(3) . . ?
N1 N2 Pd1 117.8(3) . . ?
C4 N3 N4 109.3(4) . . ?
C4 N3 B1 130.1(4) . . ?
N4 N3 B1 120.6(4) . . ?
C6 N4 N3 106.0(4) . . ?
C6 N4 Pd1 130.8(3) . . ?
N3 N4 Pd1 118.6(3) . . ?
C7 N5 N6 109.8(4) . . ?
C7 N5 B1 128.6(4) . . ?
N6 N5 B1 121.6(4) . . ?
C9 N6 N5 105.2(4) . . ?
N1 C1 C2 110.1(4) . . ?
N1 C1 Br1 122.6(4) . . ?
C2 C1 Br1 127.3(4) . . ?
C1 C2 C3 103.8(5) . . ?
C1 C2 Br2 128.5(4) . . ?
C3 C2 Br2 127.5(4) . . ?
N2 C3 C2 111.8(5) . . ?
N2 C3 Br3 121.3(4) . . ?
C2 C3 Br3 126.8(4) . . ?
N3 C4 C5 108.7(5) . . ?
N3 C4 Br4 123.3(4) . . ?
C5 C4 Br4 128.0(4) . . ?
C6 C5 C4 104.2(5) . . ?
C6 C5 Br5 128.7(4) . . ?
C4 C5 Br5 127.0(4) . . ?
N4 C6 C5 111.8(5) . . ?
N4 C6 Br6 121.4(4) . . ?
C5 C6 Br6 126.7(4) . . ?
N5 C7 C8 108.6(5) . . ?
N5 C7 Br7 123.0(4) . . ?
C8 C7 Br7 128.3(4) . . ?
C9 C8 C7 103.5(5) . . ?
C9 C8 Br8 128.9(4) . . ?
C7 C8 Br8 127.6(4) . . ?
N6 C9 C8 112.8(5) . . ?
N6 C9 Br9 118.7(4) . . ?
C8 C9 Br9 128.4(4) . . ?
C11 C10 Pd1 72.1(3) . . ?
C12 C11 C10 113.8(5) . . ?
C12 C11 C13 122.0(6) . . ?
C10 C11 C13 122.7(7) . . ?
C12 C11 Pd1 69.4(3) . . ?
C10 C11 Pd1 69.2(3) . . ?
C13 C11 Pd1 119.0(4) . . ?
C11 C12 Pd1 72.0(4) . . ?
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
Pd1 C10 2.103(6) . ?
Pd1 C12 2.107(6) . ?
Pd1 N4 2.124(4) . ?
Pd1 N2 2.127(4) . ?
Pd1 C11 2.141(5) . ?
B1 N5 1.535(8) . ?
B1 N1 1.537(7) . ?
B1 N3 1.563(7) . ?
Br1 C1 1.862(5) . ?
Br2 C2 1.857(5) . ?
Br3 C3 1.860(5) . ?
Br4 C4 1.841(5) . ?
Br5 C5 1.859(6) . ?
Br6 C6 1.861(5) . ?
Br7 C7 1.853(6) . ?
Br8 C8 1.857(5) . ?
Br9 C9 1.871(6) . ?
N1 C1 1.348(7) . ?
N1 N2 1.382(5) . ?
N2 C3 1.324(7) . ?
N3 C4 1.345(7) . ?
N3 N4 1.365(5) . ?
N4 C6 1.326(7) . ?
N5 C7 1.349(7) . ?
N5 N6 1.367(6) . ?
N6 C9 1.324(7) . ?
C1 C2 1.374(7) . ?
C2 C3 1.384(8) . ?
C4 C5 1.379(8) . ?
C5 C6 1.376(8) . ?
C7 C8 1.384(8) . ?
C8 C9 1.382(7) . ?
C10 C11 1.408(9) . ?
C11 C12 1.404(10) . ?
C11 C13 1.497(9) . ?
