#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/14/2201486.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2201486
loop_
_publ_author_name
'Meij, Anna M. M.'
'Stefanus Otto'
'Andreas Roodt'
_publ_section_title
trans-Dibromobis(1,3,5-triaza-7-phosphaadamantane-κP)palladium(II)
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m644
_journal_page_last               m646
_journal_paper_doi               10.1107/S1600536802018330
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Pd Br2 (C6 H12 N3)2]'
_chemical_formula_moiety         'C12 H24 Br2 N6 P2 Pd'
_chemical_formula_sum            'C12 H24 Br2 N6 P2 Pd'
_chemical_formula_weight         580.53
_chemical_name_systematic
;
trans-Dibromobis(1,3,5-triaza-7-phosphaadamantane)palladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.276(2)
_cell_length_b                   11.808(2)
_cell_length_c                   10.317(2)
_cell_measurement_reflns_used    2112
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.63
_cell_volume                     883.0(3)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8979
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        0
_diffrn_standards_number
'first 50 frames repeated and decay corrections applied if needed'
_exptl_absorpt_coefficient_mu    5.765
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_density_meas      2.177
_exptl_crystal_density_method    'flotation in CH~2~I~2~/C~6~H~6~'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.595
_refine_diff_density_min         -1.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0392
_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)+(0.038P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                1629
_reflns_number_total             2475
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fl6002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2201486
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pd1 0.0000 0.0000 0.5000 0.02038(12) Uani d S 1 . . Pd
Br1 0.24015(7) -0.04574(4) 0.35938(5) 0.03753(15) Uani d . 1 . . Br
P1 0.13587(14) 0.17448(8) 0.54797(11) 0.0218(2) Uani d . 1 . . P
N1 0.3616(5) 0.2889(3) 0.7321(4) 0.0273(8) Uani d . 1 . . N
N3 0.1182(5) 0.4004(3) 0.6106(3) 0.0255(8) Uani d . 1 . . N
N2 0.3900(5) 0.3393(3) 0.5020(4) 0.0290(9) Uani d . 1 . . N
C1 0.2746(6) 0.1785(3) 0.7055(4) 0.0309(10) Uani d . 1 . . C
H1A 0.1961 0.1609 0.7742 0.039(4) Uiso calc R 1 . . H
H1B 0.3697 0.1209 0.7065 0.039(4) Uiso calc R 1 . . H
C3 -0.0011(6) 0.3040(3) 0.5678(5) 0.0286(10) Uani d . 1 . . C
H3A -0.0696 0.3226 0.4856 0.039(4) Uiso calc R 1 . . H
H3B -0.0892 0.2904 0.6313 0.039(4) Uiso calc R 1 . . H
C2 0.3068(6) 0.2343(4) 0.4463(5) 0.0329(11) Uani d . 1 . . C
H2A 0.4033 0.1790 0.4371 0.039(4) Uiso calc R 1 . . H
H2B 0.2477 0.2502 0.3603 0.039(4) Uiso calc R 1 . . H
C4 0.2226(6) 0.3779(4) 0.7348(5) 0.0317(10) Uani d . 1 . . C
H4A 0.1368 0.3570 0.7976 0.039(4) Uiso calc R 1 . . H
H4B 0.2833 0.4473 0.7652 0.039(4) Uiso calc R 1 . . H
C5 0.2486(6) 0.4264(3) 0.5128(5) 0.0317(10) Uani d . 1 . . C
H5A 0.1797 0.4357 0.4286 0.039(4) Uiso calc R 1 . . H
H5B 0.3090 0.4979 0.5352 0.039(4) Uiso calc R 1 . . H
C6 0.4836(6) 0.3187(4) 0.6307(5) 0.0321(11) Uani d . 1 . . C
H6A 0.5526 0.3861 0.6581 0.039(4) Uiso calc R 1 . . H
H6B 0.5717 0.2577 0.6240 0.039(4) Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd1 0.0204(2) 0.0172(2) 0.0232(2) 0.00008(18) 0.00011(17) -0.00444(19)
Br1 0.0391(3) 0.0288(3) 0.0472(3) 0.0026(2) 0.0185(2) -0.0075(2)
P1 0.0203(5) 0.0183(5) 0.0268(6) -0.0011(4) 0.0020(5) -0.0040(4)
N1 0.031(2) 0.0189(17) 0.030(2) -0.0061(15) -0.0073(17) -0.0010(15)
N3 0.0249(18) 0.0163(17) 0.035(2) 0.0013(14) 0.0015(16) -0.0026(14)
N2 0.028(2) 0.0237(19) 0.036(2) -0.0079(15) 0.0085(18) -0.0027(16)
C1 0.034(2) 0.021(2) 0.037(3) -0.0068(18) -0.004(2) 0.0069(19)
C3 0.022(2) 0.024(2) 0.039(3) 0.0041(17) -0.002(2) -0.0033(19)
C2 0.036(3) 0.034(2) 0.031(3) -0.005(2) 0.012(2) -0.0109(19)
C4 0.039(3) 0.024(2) 0.032(3) -0.0047(19) 0.002(2) -0.0097(19)
C5 0.035(2) 0.022(2) 0.037(3) -0.0022(19) 0.000(2) 0.0061(19)
C6 0.020(2) 0.021(2) 0.054(3) -0.0010(17) -0.003(2) 0.003(2)
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'
P P 0.1023 0.0942 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 Pd1 P1 . 3_556 180.0 yes
P1 Pd1 Br1 . . 90.55(3) yes
P1 Pd1 Br1 3_556 . 89.45(3) yes
P1 Pd1 Br1 . 3_556 89.45(3) ?
P1 Pd1 Br1 3_556 3_556 90.55(3) ?
Br1 Pd1 Br1 . 3_556 180.0 ?
C2 P1 C1 . . 98.5(2) yes
C2 P1 C3 . . 98.2(2) yes
C1 P1 C3 . . 98.1(2) yes
C2 P1 Pd1 . . 121.10(10) yes
C1 P1 Pd1 . . 113.80(10) yes
C3 P1 Pd1 . . 122.40(10) yes
C4 N1 C1 . . 110.8(3) ?
C4 N1 C6 . . 107.7(3) ?
C1 N1 C6 . . 110.9(3) ?
C4 N3 C3 . . 111.8(3) ?
C4 N3 C5 . . 108.8(3) ?
C3 N3 C5 . . 110.6(3) ?
C6 N2 C5 . . 108.8(3) ?
C6 N2 C2 . . 111.0(3) ?
C5 N2 C2 . . 110.7(3) ?
N1 C1 P1 . . 112.6(3) ?
N1 C1 H1A . . 109.1 ?
P1 C1 H1A . . 109.1 ?
N1 C1 H1B . . 109.1 ?
P1 C1 H1B . . 109.1 ?
H1A C1 H1B . . 107.8 ?
N3 C3 P1 . . 111.3(3) ?
N3 C3 H3A . . 109.4 ?
P1 C3 H3A . . 109.4 ?
N3 C3 H3B . . 109.4 ?
P1 C3 H3B . . 109.4 ?
H3A C3 H3B . . 108.0 ?
N2 C2 P1 . . 112.1(3) ?
N2 C2 H2A . . 109.2 ?
P1 C2 H2A . . 109.2 ?
N2 C2 H2B . . 109.2 ?
P1 C2 H2B . . 109.2 ?
H2A C2 H2B . . 107.9 ?
N3 C4 N1 . . 115.1(3) ?
N3 C4 H4A . . 108.5 ?
N1 C4 H4A . . 108.5 ?
N3 C4 H4B . . 108.5 ?
N1 C4 H4B . . 108.5 ?
H4A C4 H4B . . 107.5 ?
N2 C5 N3 . . 113.7(3) ?
N2 C5 H5A . . 108.8 ?
N3 C5 H5A . . 108.8 ?
N2 C5 H5B . . 108.8 ?
N3 C5 H5B . . 108.8 ?
H5A C5 H5B . . 107.7 ?
N2 C6 N1 . . 115.1(3) ?
N2 C6 H6A . . 108.5 ?
N1 C6 H6A . . 108.5 ?
N2 C6 H6B . . 108.5 ?
N1 C6 H6B . . 108.5 ?
H6A C6 H6B . . 107.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 P1 . 2.3120(10) yes
Pd1 P1 3_556 2.3120(10) ?
Pd1 Br1 . 2.4270(10) yes
Pd1 Br1 3_556 2.4270(10) ?
P1 C2 . 1.836(4) yes
P1 C1 . 1.838(5) yes
P1 C3 . 1.847(4) yes
N1 C4 . 1.460(5) ?
N1 C1 . 1.465(5) ?
N1 C6 . 1.472(6) ?
N3 C4 . 1.456(6) ?
N3 C3 . 1.476(5) ?
N3 C5 . 1.477(5) ?
N2 C6 . 1.459(6) ?
N2 C5 . 1.466(5) ?
N2 C2 . 1.473(5) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
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
Br1 Pd1 P1 C1 -100.2(2)
Br1 Pd1 P1 C2 16.9(2)
Br1 Pd1 P1 C3 142.4(2)
