#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:50:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179818 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/14/7011452.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_7011452
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            'C19 H29 B N6 Pd'
_chemical_formula_weight         458.69
_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                 114.7850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0102(8)
_cell_length_b                   8.4061(4)
_cell_length_c                   17.2544(9)
_cell_measurement_reflns_used    7513
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.387
_cell_measurement_theta_min      2.6005
_cell_volume                     2108.25(18)
_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 0.832
_diffrn_measured_fraction_theta_max 0.832
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10295
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.7749
_exptl_absorpt_correction_T_min  0.7158
_exptl_absorpt_correction_type   'Empirical from SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0312
_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)+(0.0195P)²+1.8627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                3926
_reflns_number_total             4410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111568p.txt
_cod_data_source_block           6
_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.

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               7011452
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.254598(15) 0.10714(2) 0.407168(11) 0.02026(7) Uani 1 1 d . . .
N1 N 0.14314(16) 0.2351(2) 0.31937(13) 0.0205(5) Uani 1 1 d . . .
N2 N 0.13718(15) 0.2444(2) 0.23752(13) 0.0198(5) Uani 1 1 d . . .
N3 N 0.22200(16) -0.0687(2) 0.31371(13) 0.0213(5) Uani 1 1 d . . .
N4 N 0.20565(16) -0.0214(2) 0.23270(13) 0.0202(5) Uani 1 1 d . . .
N5 N 0.30547(16) 0.2248(2) 0.26923(13) 0.0213(5) Uani 1 1 d . . .
N6 N 0.31418(17) 0.3786(2) 0.29852(14) 0.0254(5) Uani 1 1 d . . .
B1 B 0.2080(2) 0.1577(3) 0.21362(18) 0.0212(6) Uani 1 1 d . . .
H1 H 0.1866(19) 0.176(3) 0.1467(17) 0.021(7) Uiso 1 1 d . . .
C1 C 0.07391(19) 0.3184(3) 0.32210(17) 0.0251(6) Uani 1 1 d . . .
C2 C 0.0216(2) 0.3825(3) 0.24156(18) 0.0289(6) Uani 1 1 d . . .
H2 H -0.0318 0.4469 0.2256 0.035 Uiso 1 1 calc R . .
C3 C 0.0629(2) 0.3341(3) 0.18992(17) 0.0250(6) Uani 1 1 d . . .
C4 C 0.0589(2) 0.3293(4) 0.40142(19) 0.0360(7) Uani 1 1 d . . .
H4A H 0.0061 0.2634 0.3955 0.054 Uiso 1 1 calc R . .
H4B H 0.0469 0.4402 0.4110 0.054 Uiso 1 1 calc R . .
H4C H 0.1140 0.2916 0.4500 0.054 Uiso 1 1 calc R . .
C5 C 0.0350(2) 0.3680(3) 0.09726(18) 0.0349(7) Uani 1 1 d . . .
H5A H 0.0839 0.4279 0.0903 0.052 Uiso 1 1 calc R . .
H5B H -0.0218 0.4307 0.0750 0.052 Uiso 1 1 calc R . .
H5C H 0.0247 0.2675 0.0658 0.052 Uiso 1 1 calc R . .
C6 C 0.2135(2) -0.2264(3) 0.31240(17) 0.0260(6) Uani 1 1 d . . .
C7 C 0.1934(2) -0.2832(3) 0.23047(18) 0.0287(6) Uani 1 1 d . . .
H7 H 0.1848 -0.3909 0.2121 0.034 Uiso 1 1 calc R . .
C8 C 0.1885(2) -0.1508(3) 0.18175(17) 0.0239(6) Uani 1 1 d . . .
C9 C 0.2199(2) -0.3185(3) 0.3887(2) 0.0384(7) Uani 1 1 d . . .
H9A H 0.2649 -0.2680 0.4406 0.058 Uiso 1 1 calc R . .
H9B H 0.2394 -0.4277 0.3849 0.058 Uiso 1 1 calc R . .
H9C H 0.1596 -0.3203 0.3906 0.058 Uiso 1 1 calc R . .
C10 C 0.1698(2) -0.1410(3) 0.08960(17) 0.0329(7) Uani 1 1 d . . .
H10A H 0.1169 -0.0712 0.0599 0.049 Uiso 1 1 calc R . .
H10B H 0.1562 -0.2475 0.0643 0.049 Uiso 1 1 calc R . .
H10C H 0.2239 -0.0980 0.0841 0.049 Uiso 1 1 calc R . .
C11 C 0.3892(2) 0.1613(3) 0.28687(18) 0.0277(6) Uani 1 1 d . . .
C12 C 0.4540(2) 0.2755(3) 0.32950(19) 0.0312(7) Uani 1 1 d . . .
H12 H 0.5189 0.2662 0.3508 0.037 Uiso 1 1 calc R . .
C13 C 0.4038(2) 0.4075(3) 0.33470(18) 0.0292(7) Uani 1 1 d . . .
C14 C 0.4046(2) -0.0034(4) 0.2624(2) 0.0451(9) Uani 1 1 d . . .
H14A H 0.3812 -0.0812 0.2908 0.068 Uiso 1 1 calc R . .
H14B H 0.4706 -0.0208 0.2801 0.068 Uiso 1 1 calc R . .
H14C H 0.3721 -0.0161 0.2004 0.068 Uiso 1 1 calc R . .
C15 C 0.4398(3) 0.5681(4) 0.3729(2) 0.0454(9) Uani 1 1 d . . .
H15A H 0.3894 0.6454 0.3529 0.068 Uiso 1 1 calc R . .
H15B H 0.4878 0.6023 0.3554 0.068 Uiso 1 1 calc R . .
H15C H 0.4656 0.5608 0.4353 0.068 Uiso 1 1 calc R . .
C16 C 0.3427(2) 0.1151(3) 0.54095(17) 0.0304(7) Uani 1 1 d . . .
C17 C 0.3140(2) 0.2697(3) 0.50918(19) 0.0337(7) Uani 1 1 d D . .
H17A H 0.348(2) 0.331(4) 0.4872(19) 0.038(9) Uiso 1 1 d D . .
H17B H 0.277(2) 0.333(4) 0.529(2) 0.050(10) Uiso 1 1 d D . .
C18 C 0.3840(2) 0.0279(4) 0.49749(18) 0.0321(7) Uani 1 1 d D . .
H18A H 0.4165(19) 0.087(3) 0.4727(18) 0.026(8) Uiso 1 1 d D . .
H18B H 0.394(2) -0.078(3) 0.509(2) 0.037(9) Uiso 1 1 d D . .
C19 C 0.3129(3) 0.0394(4) 0.60355(19) 0.0405(8) Uani 1 1 d . . .
H19A H 0.3093 -0.0762 0.5952 0.061 Uiso 1 1 calc R . .
H19B H 0.2523 0.0805 0.5948 0.061 Uiso 1 1 calc R . .
H19C H 0.3576 0.0641 0.6617 0.061 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'
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
N3 Pd1 N1 86.76(8) . . ?
N3 Pd1 C16 133.89(10) . . ?
N1 Pd1 C16 137.81(10) . . ?
C1 N1 N2 107.8(2) . . ?
C1 N1 Pd1 135.80(18) . . ?
N2 N1 Pd1 116.32(16) . . ?
C3 N2 N1 108.6(2) . . ?
C3 N2 B1 131.1(2) . . ?
N1 N2 B1 120.3(2) . . ?
C6 N3 N4 107.3(2) . . ?
C6 N3 Pd1 135.15(18) . . ?
N4 N3 Pd1 117.56(14) . . ?
C8 N4 N3 109.27(19) . . ?
C8 N4 B1 131.4(2) . . ?
N3 N4 B1 119.28(19) . . ?
C11 N5 N6 110.5(2) . . ?
C11 N5 B1 129.7(2) . . ?
N6 N5 B1 119.3(2) . . ?
C13 N6 N5 105.6(2) . . ?
N2 B1 N4 108.5(2) . . ?
N2 B1 N5 108.9(2) . . ?
N4 B1 N5 109.2(2) . . ?
N1 C1 C2 109.2(2) . . ?
N1 C1 C4 121.6(2) . . ?
C2 C1 C4 129.2(3) . . ?
C3 C2 C1 106.3(2) . . ?
N2 C3 C2 108.1(2) . . ?
N2 C3 C5 123.1(3) . . ?
C2 C3 C5 128.9(3) . . ?
N3 C6 C7 109.6(2) . . ?
N3 C6 C9 122.2(2) . . ?
C7 C6 C9 128.1(2) . . ?
C8 C7 C6 105.8(2) . . ?
N4 C8 C7 108.0(2) . . ?
N4 C8 C10 122.9(2) . . ?
C7 C8 C10 129.1(2) . . ?
N5 C11 C12 107.3(2) . . ?
N5 C11 C14 124.4(3) . . ?
C12 C11 C14 128.2(3) . . ?
C11 C12 C13 105.3(3) . . ?
N6 C13 C12 111.2(2) . . ?
N6 C13 C15 120.7(3) . . ?
C12 C13 C15 128.1(3) . . ?
C18 C16 C17 115.1(3) . . ?
C18 C16 C19 122.1(3) . . ?
C17 C16 C19 121.6(3) . . ?
C18 C16 Pd1 69.59(16) . . ?
C17 C16 Pd1 69.53(16) . . ?
C19 C16 Pd1 120.0(2) . . ?
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 N3 2.086(2) . ?
Pd1 N1 2.090(2) . ?
Pd1 C16 2.143(3) . ?
N1 C1 1.328(3) . ?
N1 N2 1.377(3) . ?
N2 C3 1.356(3) . ?
N2 B1 1.542(4) . ?
N3 C6 1.332(3) . ?
N3 N4 1.369(3) . ?
N4 C8 1.353(3) . ?
N4 B1 1.545(3) . ?
N5 C11 1.354(4) . ?
N5 N6 1.373(3) . ?
N5 B1 1.556(4) . ?
N6 C13 1.326(4) . ?
C1 C2 1.395(4) . ?
C1 C4 1.488(4) . ?
C2 C3 1.374(4) . ?
C3 C5 1.496(4) . ?
C6 C7 1.396(4) . ?
C6 C9 1.493(4) . ?
C7 C8 1.377(4) . ?
C8 C10 1.492(4) . ?
C11 C12 1.377(4) . ?
C11 C14 1.498(4) . ?
C12 C13 1.395(4) . ?
C13 C15 1.506(4) . ?
C16 C18 1.397(4) . ?
C16 C17 1.411(4) . ?
C16 C19 1.494(4) . ?
