#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:42:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179343 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324024.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_4324024
loop_
_publ_author_name
'Donald J. Darensbourg'
'Tara J. Decuir'
'Nicole White Stafford'
'Jeffrey B. Robertson'
'Jennifer D. Draper'
'Joseph H. Reibenspies'
'Agnes Kathó'
'Ferenc Joó'
_publ_section_title
;
 Water-Soluble Organometallic Compounds. 6.1Synthesis, Spectral
 Properties, and Crystal Structures of Complexes of
 1,3,5-Triaza-7-phosphaadamantane with Group 10 Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4218
_journal_page_last               4226
_journal_paper_doi               10.1021/ic970238x
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C12 H33 Cl2 N6 O6 P2 Pd'
_chemical_formula_weight         596.68
_chemical_name_systematic
;                                                                               
 ?                                                                              
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.93(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.755(7)
_cell_length_b                   7.103(3)
_cell_length_c                   14.877(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1222.3(13)
_computing_cell_refinement       'P3VAX (SIEMENS, 1990)'
_computing_data_collection       'P3VAX (SIEMENS, 1990)'
_computing_data_reduction        'XDISK (SIEMENS, 1990)'
_computing_molecular_graphics    'XP (SIEMENS, 1990)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3M'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2131
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       needle
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.568
_refine_diff_density_min         -3.258
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       0.0126(71)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.106
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.405
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_obs          0.1228
_refine_ls_shift/esd_max         -0.047
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2582P)²+15.3641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.5063
_refine_ls_wR_factor_obs         0.3249
_reflns_number_observed          1497
_reflns_number_total             2035
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970238x_4.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2582P)^2^+15.3641P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2582P)^2^+15.3641P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1222.3(12)
_cod_database_code               4324024
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pd1 Pd 0.43870(12) 0.2500 0.42088(10) 0.0522(10) Uani 1 d S .
Cl1 Cl 0.5806(4) 0.2500 0.5864(4) 0.054(2) Uani 1 d S .
Cl2 Cl 0.5850(4) 0.2500 0.3632(4) 0.057(2) Uani 1 d S .
P1 P 0.2981(4) 0.2500 0.4722(4) 0.047(2) Uani 1 d S .
P2 P 0.3164(5) 0.2500 0.2579(4) 0.066(2) Uani 1 d S .
O1 O 0.3638(56) 0.7500 0.0197(47) 0.315(31) Uiso 1 d S .
H1C H 0.3955(56) 0.7500 -0.0109(47) 0.473 Uiso 1 d SR .
H1D H 0.2823(56) 0.7500 0.0034(47) 0.473 Uiso 1 d SR .
O2 O 0.0689(14) 0.7500 0.2098(8) 0.069(5) Uani 1 d S .
H2C H 0.0082(14) 0.7500 0.2201(8) 0.010(38) Uiso 1 d SR .
O3 O -0.1090(14) 0.4549 0.2103(8) 0.244(15) Uiso 1 d R .
H3B H -0.1408(14) 0.4932 0.2470(8) 0.366 Uiso 1 d R .
H3C H -0.1603(14) 0.4393 0.1516(8) 0.366 Uiso 1 d R .
O4 O 0.3678(33) 0.4380(61) 0.8281(28) 0.284(19) Uiso 1 d . .
H4E H 0.3445(33) 0.3598(61) 0.8590(28) 0.426 Uiso 1 d R .
H4F H 0.4346(33) 0.4059(61) 0.8340(28) 0.426 Uiso 1 d R .
N1 N 0.1141(10) 0.4241(21) 0.4862(9) 0.057(3) Uani 1 d . .
N2 N 0.2474(13) 0.2500 0.6301(13) 0.047(4) Uani 1 d S .
N3 N 0.2710(13) 0.4218(28) 0.0810(10) 0.081(5) Uani 1 d . .
N4 N 0.1114(17) 0.2500 0.0918(16) 0.083(7) Uani 1 d S .
C1 C 0.1958(11) 0.4482(25) 0.4415(10) 0.050(4) Uani 1 d . .
H1A H 0.2387(11) 0.5644(25) 0.4652(10) 0.075 Uiso 1 d R .
H1B H 0.1536(11) 0.4573(25) 0.3701(10) 0.075 Uiso 1 d R .
C2 C 0.1748(14) 0.4176(35) 0.5953(12) 0.077(6) Uani 1 d . .
H2A H 0.1181(14) 0.4210(35) 0.6228(12) 0.116 Uiso 1 d R .
H2B H 0.2232(14) 0.5284(35) 0.6185(12) 0.116 Uiso 1 d R .
C3 C 0.3516(18) 0.2500 0.6091(17) 0.065(7) Uani 1 d S .
H3A H 0.3978(18) 0.3598 0.6369(17) 0.078 Uiso 0.50 d PR .
C4 C 0.0485(17) 0.2500 0.4511(16) 0.064(7) Uani 1 d S .
H4A H 0.0147(17) 0.2500 0.3792(16) 0.097 Uiso 1 d SR .
H4B H -0.0146(17) 0.2500 0.4713(16) 0.097 Uiso 1 d SR .
C4 C 0.3378(15) 0.4459(32) 0.1894(11) 0.074(5) Uani 1 d . .
H4C H 0.3139(15) 0.5610(32) 0.2105(11) 0.111 Uiso 1 d R .
H4D H 0.4194(15) 0.4569(32) 0.2048(11) 0.111 Uiso 1 d R .
C5 C 0.1432(18) 0.4138(44) 0.0523(14) 0.106(9) Uani 1 d . .
H5A H 0.1194(18) 0.5254(44) 0.0764(14) 0.159 Uiso 1 d R .
H5B H 0.1031(18) 0.4133(44) -0.0194(14) 0.159 Uiso 1 d R .
C6 C 0.1535(20) 0.2500 0.1987(18) 0.087(10) Uani 1 d S .
H6A H 0.1255(20) 0.3595 0.2195(18) 0.104 Uiso 0.50 d PR .
C7 C 0.3022(24) 0.2500 0.0462(19) 0.091(10) Uani 1 d S .
H7A H 0.3851(24) 0.2500 0.0660(19) 0.137 Uiso 1 d SR .
H7B H 0.2649(24) 0.2500 -0.0257(19) 0.137 Uiso 1 d SR .
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
P1 Pd1 P2 94.4(2) . . ?
P1 Pd1 Cl2 178.9(2) . . ?
P2 Pd1 Cl2 84.5(2) . . ?
P1 Pd1 Cl1 90.9(2) . . ?
P2 Pd1 Cl1 174.7(2) . . ?
Cl2 Pd1 Cl1 90.2(2) . . ?
C1 P1 C1 99.8(10) 4_565 . ?
C1 P1 C3 99.6(6) 4_565 . ?
C1 P1 C3 99.6(6) . . ?
C1 P1 Pd1 120.3(5) 4_565 . ?
C1 P1 Pd1 120.3(5) . . ?
C3 P1 Pd1 113.6(7) . . ?
C4 P2 C4 100.4(13) 4_565 . ?
C4 P2 C6 97.8(8) 4_565 . ?
C4 P2 C6 97.8(8) . . ?
C4 P2 Pd1 113.8(6) 4_565 . ?
C4 P2 Pd1 113.8(6) . . ?
C6 P2 Pd1 128.8(8) . . ?
C4 N1 C1 110.4(14) . . ?
C4 N1 C2 108.8(15) . . ?
C1 N1 C2 111.1(11) . . ?
C2 N2 C2 108.9(19) 4_565 . ?
C2 N2 C3 114.4(11) 4_565 . ?
C2 N2 C3 114.4(11) . . ?
C7 N3 C4 111.6(17) . . ?
C7 N3 C5 107.2(20) . . ?
C4 N3 C5 111.8(14) . . ?
C5 N4 C5 108.2(24) 4_565 . ?
C5 N4 C6 114.2(13) 4_565 . ?
C5 N4 C6 114.2(13) . . ?
N1 C1 P1 111.3(11) . . ?
N2 C2 N1 112.1(16) . . ?
N2 C3 P1 106.4(14) . . ?
N1 C4 N1 115.7(16) . 4_565 ?
N3 C4 P2 111.7(14) . . ?
N4 C5 N3 112.0(19) . . ?
N4 C6 P2 109.7(16) . . ?
N3 C7 N3 115.1(22) 4_565 . ?
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 P1 2.226(5) . ?
Pd1 P2 2.264(6) . ?
Pd1 Cl2 2.360(5) . ?
Pd1 Cl1 2.363(5) . ?
P1 C1 1.841(15) 4_565 ?
P1 C1 1.841(15) . ?
P1 C3 1.85(2) . ?
P2 C4 1.81(2) 4_565 ?
P2 C4 1.81(2) . ?
P2 C6 1.88(2) . ?
N1 C4 1.46(2) . ?
N1 C1 1.46(2) . ?
N1 C2 1.48(2) . ?
N2 C2 1.46(2) 4_565 ?
N2 C2 1.46(2) . ?
N2 C3 1.49(3) . ?
N3 C7 1.45(2) . ?
N3 C4 1.48(2) . ?
N3 C5 1.50(3) . ?
N4 C5 1.44(3) 4_565 ?
N4 C5 1.44(3) . ?
N4 C6 1.45(3) . ?
C4 N1 1.46(2) 4_565 ?
C7 N3 1.45(2) 4_565 ?
