#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:56:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179162 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/23/4312316.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_4312316
loop_
_publ_author_name
'Donald J. Darensbourg'
'Cesar G. Ortiz'
'Jason C. Yarbrough'
_publ_section_title
;
 Synthesis and Structures of Nickel and Palladium Salicylaldiminato
 1,3,5-Triaza-7-phosphaadamantane (PTA) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6915
_journal_page_last               6922
_journal_paper_doi               10.1021/ic0341284
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C30 H39 N4 O P Pd'
_chemical_formula_weight         609.02
_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                115.773(2)
_cell_angle_beta                 102.892(2)
_cell_angle_gamma                102.128(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8304(11)
_cell_length_b                   12.8719(13)
_cell_length_c                   13.2710(14)
_cell_measurement_temperature    110(2)
_cell_volume                     1380.9(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      110(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6284
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         3946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0128P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                3323
_reflns_number_total             3946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0341284si20030205_021052_8.cif
_cod_data_source_block           Structure6c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               4312316
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 0.63322(3) 0.75161(2) -0.00235(2) 0.01627(9) Uani 1 1 d . . .
P1 P 0.46002(11) 0.67003(8) -0.18026(8) 0.0166(2) Uani 1 1 d . . .
O1 O 0.6279(3) 0.57643(19) -0.04037(19) 0.0179(6) Uani 1 1 d . . .
N1 N 0.7996(3) 0.8214(2) 0.1613(2) 0.0137(7) Uani 1 1 d . . .
N2 N 0.3954(3) 0.6116(2) -0.4166(2) 0.0198(7) Uani 1 1 d . . .
N3 N 0.1944(3) 0.6380(2) -0.3344(2) 0.0173(7) Uani 1 1 d . . .
N4 N 0.2641(3) 0.4525(2) -0.3797(2) 0.0178(7) Uani 1 1 d . . .
C1 C 0.6273(4) 0.9191(3) 0.0292(3) 0.0275(10) Uani 1 1 d . . .
H1A H 0.6085 0.9208 -0.0441 0.041 Uiso 1 1 calc R . .
H1B H 0.7212 0.9815 0.0869 0.041 Uiso 1 1 calc R . .
H1C H 0.5494 0.9344 0.0597 0.041 Uiso 1 1 calc R . .
C2 C 0.8715(4) 0.7562(3) 0.1863(3) 0.0152(8) Uani 1 1 d . . .
H2 H 0.9452 0.7986 0.2620 0.018 Uiso 1 1 calc R . .
C3 C 0.8549(4) 0.6299(3) 0.1156(3) 0.0125(8) Uani 1 1 d . . .
C4 C 0.9654(4) 0.5852(3) 0.1583(3) 0.0131(8) Uani 1 1 d . . .
C5 C 0.9417(4) 0.4569(3) 0.0972(3) 0.0161(9) Uani 1 1 d . . .
C6 C 0.8097(4) 0.3769(3) -0.0036(3) 0.0184(9) Uani 1 1 d . . .
H6 H 0.7927 0.2929 -0.0431 0.022 Uiso 1 1 calc R . .
C7 C 0.7075(4) 0.4182(3) -0.0446(3) 0.0173(9) Uani 1 1 d . . .
H7 H 0.6212 0.3618 -0.1100 0.021 Uiso 1 1 calc R . .
C8 C 0.7287(4) 0.5477(3) 0.0105(3) 0.0137(8) Uani 1 1 d . . .
C9 C 0.8425(4) 0.9444(3) 0.2611(3) 0.0148(8) Uani 1 1 d . . .
C10 C 0.9612(4) 1.0392(3) 0.2778(3) 0.0172(9) Uani 1 1 d . . .
C11 C 1.0080(4) 1.1527(3) 0.3805(3) 0.0209(9) Uani 1 1 d . . .
H11 H 1.0884 1.2166 0.3945 0.025 Uiso 1 1 calc R . .
C12 C 0.9379(4) 1.1731(3) 0.4627(3) 0.0220(9) Uani 1 1 d . . .
H12 H 0.9734 1.2492 0.5328 0.026 Uiso 1 1 calc R . .
C13 C 0.8154(4) 1.0810(3) 0.4412(3) 0.0213(9) Uani 1 1 d . . .
H13 H 0.7662 1.0969 0.4955 0.026 Uiso 1 1 calc R . .
C14 C 0.7634(4) 0.9645(3) 0.3397(3) 0.0180(9) Uani 1 1 d . . .
C15 C 0.6272(4) 0.8656(3) 0.3173(3) 0.0227(9) Uani 1 1 d . . .
H15 H 0.6070 0.7924 0.2406 0.027 Uiso 1 1 calc R . .
C16 C 0.6508(4) 0.8297(3) 0.4123(3) 0.0396(11) Uani 1 1 d . . .
H16A H 0.7340 0.8018 0.4158 0.059 Uiso 1 1 calc R . .
H16B H 0.5630 0.7648 0.3930 0.059 Uiso 1 1 calc R . .
H16C H 0.6703 0.8997 0.4887 0.059 Uiso 1 1 calc R . .
C17 C 0.4917(4) 0.9054(3) 0.3059(3) 0.0345(11) Uani 1 1 d . . .
H17A H 0.5097 0.9790 0.3789 0.052 Uiso 1 1 calc R . .
H17B H 0.4061 0.8411 0.2909 0.052 Uiso 1 1 calc R . .
H17C H 0.4738 0.9212 0.2407 0.052 Uiso 1 1 calc R . .
C18 C 1.0371(4) 1.0182(3) 0.1860(3) 0.0212(9) Uani 1 1 d . . .
H18 H 0.9701 0.9429 0.1113 0.025 Uiso 1 1 calc R . .
C19 C 1.0637(4) 1.1232(3) 0.1594(3) 0.0304(10) Uani 1 1 d . . .
H19A H 1.1276 1.1987 0.2315 0.046 Uiso 1 1 calc R . .
H19B H 0.9702 1.1310 0.1297 0.046 Uiso 1 1 calc R . .
H19C H 1.1099 1.1060 0.1003 0.046 Uiso 1 1 calc R . .
C20 C 1.1815(4) 0.9981(3) 0.2251(3) 0.0345(11) Uani 1 1 d . . .
H20A H 1.2503 1.0711 0.2976 0.052 Uiso 1 1 calc R . .
H20B H 1.2237 0.9803 0.1634 0.052 Uiso 1 1 calc R . .
H20C H 1.1623 0.9302 0.2391 0.052 Uiso 1 1 calc R . .
C21 C 0.2917(4) 0.7107(3) -0.2077(3) 0.0197(9) Uani 1 1 d . . .
H21A H 0.2367 0.6972 -0.1596 0.024 Uiso 1 1 calc R . .
H21B H 0.3212 0.7975 -0.1827 0.024 Uiso 1 1 calc R . .
C22 C 0.3706(4) 0.5021(3) -0.2586(3) 0.0174(9) Uani 1 1 d . . .
H22A H 0.4466 0.4647 -0.2642 0.021 Uiso 1 1 calc R . .
H22B H 0.3189 0.4803 -0.2125 0.021 Uiso 1 1 calc R . .
C23 C 0.5171(4) 0.6808(3) -0.2993(3) 0.0189(9) Uani 1 1 d . . .
H23A H 0.5536 0.7667 -0.2771 0.023 Uiso 1 1 calc R . .
H23B H 0.5984 0.6498 -0.3060 0.023 Uiso 1 1 calc R . .
C24 C 0.3385(4) 0.4802(3) -0.4539(3) 0.0207(9) Uani 1 1 d . . .
H24A H 0.2688 0.4352 -0.5359 0.025 Uiso 1 1 calc R . .
H24B H 0.4211 0.4501 -0.4530 0.025 Uiso 1 1 calc R . .
C25 C 0.2723(4) 0.6578(3) -0.4101(3) 0.0213(9) Uani 1 1 d . . .
H25A H 0.2004 0.6189 -0.4907 0.026 Uiso 1 1 calc R . .
H25B H 0.3105 0.7455 -0.3806 0.026 Uiso 1 1 calc R . .
C26 C 0.1467(4) 0.5057(3) -0.3751(3) 0.0206(9) Uani 1 1 d . . .
H26A H 0.1010 0.4922 -0.3221 0.025 Uiso 1 1 calc R . .
H26B H 0.0707 0.4616 -0.4545 0.025 Uiso 1 1 calc R . .
C27 C 1.0994(4) 0.6611(3) 0.2561(3) 0.0164(8) Uani 1 1 d . . .
H27 H 1.1204 0.7458 0.2961 0.020 Uiso 1 1 calc R . .
C28 C 1.2006(4) 0.6159(3) 0.2952(3) 0.0215(9) Uani 1 1 d . . .
H28 H 1.2868 0.6693 0.3618 0.026 Uiso 1 1 calc R . .
C29 C 1.1744(4) 0.4901(3) 0.2355(3) 0.0223(9) Uani 1 1 d . . .
H29 H 1.2426 0.4590 0.2622 0.027 Uiso 1 1 calc R . .
C30 C 1.0481(4) 0.4126(3) 0.1375(3) 0.0212(9) Uani 1 1 d . . .
H30 H 1.0321 0.3288 0.0966 0.025 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'
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'
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
C1 Pd1 O1 177.06(13) . . ?
C1 Pd1 N1 94.15(13) . . ?
O1 Pd1 N1 88.47(10) . . ?
C1 Pd1 P1 88.23(11) . . ?
O1 Pd1 P1 89.18(7) . . ?
N1 Pd1 P1 177.27(8) . . ?
C22 P1 C23 98.02(15) . . ?
C22 P1 C21 98.75(16) . . ?
C23 P1 C21 97.61(15) . . ?
C22 P1 Pd1 114.87(11) . . ?
C23 P1 Pd1 118.21(11) . . ?
C21 P1 Pd1 124.54(11) . . ?
C8 O1 Pd1 127.2(2) . . ?
C2 N1 C9 113.1(3) . . ?
C2 N1 Pd1 123.1(2) . . ?
C9 N1 Pd1 123.8(2) . . ?
C25 N2 C23 110.3(3) . . ?
C25 N2 C24 108.0(3) . . ?
C23 N2 C24 110.4(3) . . ?
C25 N3 C21 111.0(3) . . ?
C25 N3 C26 107.5(3) . . ?
C21 N3 C26 110.6(3) . . ?
C26 N4 C24 107.9(3) . . ?
C26 N4 C22 110.9(3) . . ?
C24 N4 C22 111.0(3) . . ?
N1 C2 C3 130.2(3) . . ?
C8 C3 C2 121.1(3) . . ?
C8 C3 C4 120.2(3) . . ?
C2 C3 C4 118.6(3) . . ?
C27 C4 C5 116.3(3) . . ?
C27 C4 C3 124.2(3) . . ?
C5 C4 C3 119.5(3) . . ?
C30 C5 C6 121.6(3) . . ?
C30 C5 C4 120.0(3) . . ?
C6 C5 C4 118.4(3) . . ?
C7 C6 C5 122.4(3) . . ?
C6 C7 C8 121.7(3) . . ?
O1 C8 C3 126.3(3) . . ?
O1 C8 C7 116.0(3) . . ?
C3 C8 C7 117.7(3) . . ?
C10 C9 C14 121.9(3) . . ?
C10 C9 N1 119.7(3) . . ?
C14 C9 N1 118.4(3) . . ?
C11 C10 C9 117.8(3) . . ?
C11 C10 C18 121.0(3) . . ?
C9 C10 C18 121.1(3) . . ?
C12 C11 C10 121.4(3) . . ?
C13 C12 C11 120.0(3) . . ?
C12 C13 C14 121.4(3) . . ?
C13 C14 C9 117.3(3) . . ?
C13 C14 C15 120.3(3) . . ?
C9 C14 C15 122.4(3) . . ?
C14 C15 C16 112.3(3) . . ?
C14 C15 C17 110.7(3) . . ?
C16 C15 C17 110.9(3) . . ?
C20 C18 C10 111.4(3) . . ?
C20 C18 C19 110.6(3) . . ?
C10 C18 C19 111.9(3) . . ?
N3 C21 P1 112.1(2) . . ?
N4 C22 P1 112.3(2) . . ?
N2 C23 P1 113.0(2) . . ?
N4 C24 N2 115.0(3) . . ?
N2 C25 N3 115.6(3) . . ?
N4 C26 N3 115.7(3) . . ?
C28 C27 C4 122.7(3) . . ?
C27 C28 C29 120.0(4) . . ?
C30 C29 C28 119.6(4) . . ?
C29 C30 C5 121.3(3) . . ?
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 C1 2.026(3) . ?
Pd1 O1 2.072(2) . ?
Pd1 N1 2.074(3) . ?
Pd1 P1 2.2080(10) . ?
P1 C22 1.834(3) . ?
P1 C23 1.840(3) . ?
P1 C21 1.845(4) . ?
O1 C8 1.283(4) . ?
N1 C2 1.303(4) . ?
N1 C9 1.444(4) . ?
N2 C25 1.460(4) . ?
N2 C23 1.470(4) . ?
N2 C24 1.473(4) . ?
N3 C25 1.465(4) . ?
N3 C21 1.469(4) . ?
N3 C26 1.470(4) . ?
N4 C26 1.461(4) . ?
N4 C24 1.466(4) . ?
N4 C22 1.470(4) . ?
C2 C3 1.430(4) . ?
C3 C8 1.413(4) . ?
C3 C4 1.451(5) . ?
C4 C27 1.403(4) . ?
C4 C5 1.425(4) . ?
C5 C30 1.404(5) . ?
C5 C6 1.414(5) . ?
C6 C7 1.348(5) . ?
C7 C8 1.443(4) . ?
C9 C10 1.397(4) . ?
C9 C14 1.404(4) . ?
C10 C11 1.383(4) . ?
C10 C18 1.521(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.374(4) . ?
C13 C14 1.392(4) . ?
C14 C15 1.510(4) . ?
C15 C16 1.510(5) . ?
C15 C17 1.525(5) . ?
C18 C20 1.515(5) . ?
C18 C19 1.527(4) . ?
C27 C28 1.369(5) . ?
C28 C29 1.391(4) . ?
C29 C30 1.363(5) . ?
