#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:45:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179456 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/53/4335359.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_4335359
loop_
_publ_author_name
'Arvind K. Gupta'
'S. Arun Dixith Reddy'
'Ramamoorthy Boomishankar'
_publ_section_title
;
 Facile Formation of Stable Tris(imido)phosphate Trianions as Their Tri-
 and Hexanuclear Pd(II) Complexes in Protic Solvents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7614
_journal_paper_doi               10.1021/ic400686e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C18 H36 N3 O7 P Pd3'
_chemical_formula_weight         756.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.899(2)
_cell_length_b                   17.194(3)
_cell_length_c                   9.5281(14)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      3.19
_cell_volume                     2604.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16776
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3256
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0131P)²+3.1676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                3201
_reflns_number_total             3256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400686e_5.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        2604.8(7)
_cod_database_code               4335359
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.912077(11) 0.727373(11) 0.72310(3) 0.02252(5) Uani 1 1 d .
Pd2 Pd 1.0000 0.667967(19) 0.95577(3) 0.02329(7) Uani 1 2 d S
P1 P 1.0000 0.82350(6) 0.89861(10) 0.01948(19) Uani 1 2 d S
O1 O 1.0000 0.90128(16) 0.9618(4) 0.0320(6) Uani 1 2 d S
N1 N 0.92002(14) 0.76045(13) 0.9306(3) 0.0222(5) Uani 1 1 d .
N2 N 1.0000 0.81529(16) 0.7209(4) 0.0196(5) Uani 1 2 d S
C11 C 0.84625(18) 0.78249(17) 1.0255(3) 0.0254(6) Uani 1 1 d .
C12 C 0.7872(2) 0.7132(2) 1.0415(4) 0.0404(8) Uani 1 1 d .
H12A H 0.7408 0.7272 1.1042 0.061 Uiso 1 1 calc R
H12B H 0.8182 0.6691 1.0812 0.061 Uiso 1 1 calc R
H12C H 0.7647 0.6987 0.9494 0.061 Uiso 1 1 calc R
C13 C 0.8791(2) 0.8049(2) 1.1699(3) 0.0375(7) Uani 1 1 d .
H13A H 0.9153 0.8508 1.1618 0.056 Uiso 1 1 calc R
H13B H 0.9115 0.7616 1.2092 0.056 Uiso 1 1 calc R
H13C H 0.8316 0.8167 1.2319 0.056 Uiso 1 1 calc R
C14 C 0.7989(2) 0.84918(18) 0.9597(4) 0.0378(7) Uani 1 1 d .
H14A H 0.8361 0.8945 0.9523 0.057 Uiso 1 1 calc R
H14B H 0.7503 0.8623 1.0182 0.057 Uiso 1 1 calc R
H14C H 0.7797 0.8341 0.8659 0.057 Uiso 1 1 calc R
C21 C 1.0000 0.8865(2) 0.6248(4) 0.0272(8) Uani 1 2 d S
C23 C 0.9214(2) 0.93450(19) 0.6537(4) 0.0385(8) Uani 1 1 d .
H23A H 0.8713 0.9032 0.6334 0.058 Uiso 1 1 calc R
H23B H 0.9216 0.9808 0.5938 0.058 Uiso 1 1 calc R
H23C H 0.9207 0.9503 0.7525 0.058 Uiso 1 1 calc R
C22 C 1.0000 0.8596(3) 0.4738(5) 0.0467(13) Uani 1 2 d S
H22A H 0.9978 0.9050 0.4116 0.070 Uiso 1 2 calc SR
H22B H 0.9508 0.8266 0.4570 0.070 Uiso 0.50 1 calc PR
H22C H 1.0514 0.8300 0.4550 0.070 Uiso 0.50 1 calc PR
C1 C 0.8555(2) 0.5789(2) 0.8449(5) 0.0458(9) Uani 1 1 d .
C2 C 0.7995(3) 0.5088(3) 0.8423(7) 0.0843(19) Uani 1 1 d .
H2A H 0.7408 0.5254 0.8340 0.127 Uiso 1 1 calc R
H2B H 0.8069 0.4792 0.9293 0.127 Uiso 1 1 calc R
H2C H 0.8143 0.4760 0.7619 0.127 Uiso 1 1 calc R
O2 O 0.91176(13) 0.58110(13) 0.9400(3) 0.0419(6) Uani 1 1 d .
O3 O 0.84041(15) 0.63011(13) 0.7520(3) 0.0376(6) Uani 1 1 d .
C3 C 1.0000 0.6665(3) 0.4733(5) 0.0315(10) Uani 1 2 d S
C4 C 1.0000 0.6174(3) 0.3428(5) 0.0471(13) Uani 1 2 d S
H4A H 0.9546 0.6344 0.2804 0.071 Uiso 0.50 1 calc PR
H4B H 0.9913 0.5627 0.3682 0.071 Uiso 0.50 1 calc PR
H4C H 1.0541 0.6229 0.2945 0.071 Uiso 0.50 1 calc PR
O4 O 0.92906(15) 0.68474(13) 0.5233(2) 0.0335(5) Uani 1 1 d .
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
O3 Pd1 O4 84.62(9) . .
O3 Pd1 N2 168.90(11) . .
O4 Pd1 N2 99.39(13) . .
O3 Pd1 N1 97.51(9) . .
O4 Pd1 N1 167.87(9) . .
N2 Pd1 N1 76.44(12) . .
O3 Pd1 P1 134.23(7) . .
O4 Pd1 P1 135.54(7) . .
N2 Pd1 P1 38.33(11) . .
N1 Pd1 P1 38.33(6) . .
O3 Pd1 Pd1 123.91(7) . 4_755
O4 Pd1 Pd1 82.46(6) . 4_755
N2 Pd1 Pd1 47.24(5) . 4_755
N1 Pd1 Pd1 86.49(6) . 4_755
P1 Pd1 Pd1 59.267(12) . 4_755
O3 Pd1 Pd2 82.74(7) . .
O4 Pd1 Pd2 122.32(7) . .
N2 Pd1 Pd2 86.39(9) . .
N1 Pd1 Pd2 46.66(6) . .
P1 Pd1 Pd2 58.91(2) . .
Pd1 Pd1 Pd2 60.199(7) 4_755 .
N1 Pd2 N1 76.67(13) . 4_755
N1 Pd2 O2 168.19(10) . 4_755
N1 Pd2 O2 97.57(9) 4_755 4_755
N1 Pd2 O2 97.57(9) . .
N1 Pd2 O2 168.20(10) 4_755 .
O2 Pd2 O2 86.13(13) 4_755 .
N1 Pd2 P1 38.43(6) . .
N1 Pd2 P1 38.43(6) 4_755 .
O2 Pd2 P1 134.25(6) 4_755 .
O2 Pd2 P1 134.25(6) . .
N1 Pd2 Pd1 86.25(7) . 4_755
N1 Pd2 Pd1 47.00(7) 4_755 4_755
O2 Pd2 Pd1 82.36(7) 4_755 4_755
O2 Pd2 Pd1 123.08(8) . 4_755
P1 Pd2 Pd1 59.129(18) . 4_755
N1 Pd2 Pd1 47.00(7) . .
N1 Pd2 Pd1 86.25(7) 4_755 .
O2 Pd2 Pd1 123.08(8) 4_755 .
O2 Pd2 Pd1 82.36(7) . .
P1 Pd2 Pd1 59.129(18) . .
Pd1 Pd2 Pd1 59.600(14) 4_755 .
O1 P1 N1 120.54(11) . 4_755
O1 P1 N1 120.55(11) . .
N1 P1 N1 96.94(16) 4_755 .
O1 P1 N2 119.00(18) . .
N1 P1 N2 97.24(11) 4_755 .
N1 P1 N2 97.24(11) . .
O1 P1 Pd2 144.25(15) . .
N1 P1 Pd2 48.61(8) 4_755 .
N1 P1 Pd2 48.61(8) . .
N2 P1 Pd2 96.74(10) . .
O1 P1 Pd1 143.32(8) . 4_755
N1 P1 Pd1 48.82(9) 4_755 4_755
N1 P1 Pd1 96.13(9) . 4_755
N2 P1 Pd1 48.74(7) . 4_755
Pd2 P1 Pd1 61.96(2) . 4_755
O1 P1 Pd1 143.32(8) . .
N1 P1 Pd1 96.13(9) 4_755 .
N1 P1 Pd1 48.82(9) . .
N2 P1 Pd1 48.74(7) . .
Pd2 P1 Pd1 61.96(2) . .
Pd1 P1 Pd1 61.47(2) 4_755 .
C11 N1 P1 121.49(19) . .
C11 N1 Pd2 126.82(17) . .
P1 N1 Pd2 92.96(10) . .
C11 N1 Pd1 126.06(17) . .
P1 N1 Pd1 92.84(11) . .
Pd2 N1 Pd1 86.33(9) . .
C21 N2 P1 122.0(2) . .
C21 N2 Pd1 126.43(17) . .
P1 N2 Pd1 92.93(14) . .
C21 N2 Pd1 126.43(17) . 4_755
P1 N2 Pd1 92.93(14) . 4_755
Pd1 N2 Pd1 85.51(10) . 4_755
C14 C11 C13 110.8(3) . .
C14 C11 C12 109.2(3) . .
C13 C11 C12 108.6(3) . .
C14 C11 N1 109.0(2) . .
C13 C11 N1 109.5(2) . .
C12 C11 N1 109.7(2) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C22 C21 C23 109.7(2) . 4_755
C22 C21 C23 109.7(2) . .
C23 C21 C23 110.3(4) 4_755 .
C22 C21 N2 109.0(3) . .
C23 C21 N2 109.0(2) 4_755 .
C23 C21 N2 109.0(2) . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
O3 C1 O2 127.4(3) . .
O3 C1 C2 115.7(4) . .
O2 C1 C2 117.0(4) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 O2 Pd2 123.6(2) . .
C1 O3 Pd1 123.8(2) . .
O4 C3 O4 126.3(4) . 4_755
O4 C3 C4 116.8(2) . .
O4 C3 C4 116.8(2) 4_755 .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 O4 Pd1 123.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O3 2.042(2) .
Pd1 O4 2.058(2) .
Pd1 N2 2.059(2) .
Pd1 N1 2.061(3) .
Pd1 P1 2.7355(9) .
Pd1 Pd1 2.7958(6) 4_755
Pd1 Pd2 2.8129(5) .
Pd2 N1 2.050(2) .
Pd2 N1 2.050(2) 4_755
Pd2 O2 2.055(2) 4_755
Pd2 O2 2.055(2) .
Pd2 P1 2.7292(11) .
Pd2 Pd1 2.8128(5) 4_755
P1 O1 1.467(3) .
P1 N1 1.699(2) 4_755
P1 N1 1.699(2) .
P1 N2 1.699(4) .
P1 Pd1 2.7355(9) 4_755
N1 C11 1.528(4) .
N2 C21 1.529(5) .
N2 Pd1 2.059(2) 4_755
C11 C14 1.508(4) .
C11 C13 1.522(4) .
C11 C12 1.525(4) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C21 C22 1.511(6) .
C21 C23 1.523(4) 4_755
C21 C23 1.523(4) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C1 O3 1.272(4) .
C1 O2 1.274(5) .
C1 C2 1.498(5) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 O4 1.264(3) .
C3 O4 1.264(3) 4_755
C3 C4 1.503(7) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
