#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320480.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_4320480
loop_
_publ_author_name
'Savariraj Kingsley'
'Vadapalli Chandrasekhar'
'Christopher D. Incarvito'
'Matthew K. Lam'
'Arnold L. Rheingold'
_publ_contact_author
;
       Chandrasekhar. V
       Department of Chemistry
       IIT, Kanpur 208 016
       India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91 512 597 436'
_publ_contact_author_phone       '+91 512 597 617'
_publ_section_title
;
 Tethered Pyrazolyl Phosphinate: Pyrazolyl-N- and Phosphoryl-O-Metal
 Coordination in Ph2P(O){OCH2CH2(3,5-Me2Pz)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5896
_journal_paper_doi               10.1021/ic010454c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C38 H42 Cl2 N4 O4 P2 Pd'
_chemical_formula_sum            'C38 H42 Cl2 N4 O4 P2 Pd'
_chemical_formula_weight         858.02
_chemical_melting_point          170
_chemical_name_common            Pdopp2epz(5)
_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                97.551(18)
_cell_angle_beta                 90.000(10)
_cell_angle_gamma                106.87(8)
_cell_formula_units_Z            1
_cell_length_a                   7.671(16)
_cell_length_b                   11.487(2)
_cell_length_c                   11.763(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     983(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3717
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                3215
_reflns_number_total             3433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010454c_5.cif
_cod_data_source_block           PdOPP2EPZ
_cod_original_cell_volume        982(2)
_cod_database_code               4320480
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
C9 C 0.6586(6) -0.3866(4) 1.6712(3) 0.0667(10) Uani 1 1 d . . .
H9 H 0.6844 -0.4212 1.7340 0.080 Uiso 1 1 calc R . .
C10 C 0.4828(6) -0.3822(4) 1.6510(4) 0.0663(10) Uani 1 1 d . . .
H10 H 0.3906 -0.4147 1.6993 0.080 Uiso 1 1 calc R . .
C8 C 0.7944(5) -0.3405(3) 1.5999(3) 0.0552(8) Uani 1 1 d . . .
H8 H 0.9116 -0.3447 1.6138 0.066 Uiso 1 1 calc R . .
C11 C 0.4456(5) -0.3293(4) 1.5589(4) 0.0619(9) Uani 1 1 d . . .
H11 H 0.3283 -0.3250 1.5457 0.074 Uiso 1 1 calc R . .
C3 C 0.9530(7) -0.5137(4) 1.1715(4) 0.0833(14) Uani 1 1 d . . .
H3 H 1.0178 -0.5710 1.1602 0.100 Uiso 1 1 calc R . .
C4 C 0.8172(8) -0.5178(4) 1.0946(4) 0.0852(16) Uani 1 1 d . . .
H4 H 0.7900 -0.5785 1.0312 0.102 Uiso 1 1 calc R . .
C2 C 0.9942(6) -0.4232(4) 1.2672(4) 0.0649(10) Uani 1 1 d . . .
H2 H 1.0870 -0.4193 1.3197 0.078 Uiso 1 1 calc R . .
C7 C 0.7579(4) -0.2872(3) 1.5063(3) 0.0411(6) Uani 1 1 d . . .
C12 C 0.5813(5) -0.2829(3) 1.4864(3) 0.0550(8) Uani 1 1 d . . .
H12 H 0.5548 -0.2485 1.4236 0.066 Uiso 1 1 calc R . .
C5 C 0.7218(7) -0.4352(4) 1.1091(3) 0.0763(13) Uani 1 1 d . . .
H5 H 0.6305 -0.4391 1.0555 0.092 Uiso 1 1 calc R . .
C1 C 0.8955(4) -0.3392(3) 1.2831(3) 0.0440(7) Uani 1 1 d . . .
C6 C 0.7600(5) -0.3436(3) 1.2049(3) 0.0559(9) Uani 1 1 d . . .
H6 H 0.6945 -0.2866 1.2152 0.067 Uiso 1 1 calc R . .
O1 O 1.1217(3) -0.2106(2) 1.4643(2) 0.0519(5) Uani 1 1 d . . .
P1 P 0.93861(10) -0.23188(7) 1.41282(6) 0.0379(2) Uani 1 1 d . . .
O2 O 0.8923(3) -0.11323(19) 1.38163(17) 0.0416(5) Uani 1 1 d . . .
C15 C 0.5206(5) -0.0178(4) 1.3470(3) 0.0564(9) Uani 1 1 d . . .
H15A H 0.6251 0.0309 1.3942 0.085 Uiso 1 1 calc R . .
H15B H 0.4628 -0.0907 1.3803 0.085 Uiso 1 1 calc R . .
H15C H 0.4361 0.0289 1.3419 0.085 Uiso 1 1 calc R . .
C17 C 0.4814(4) -0.1211(3) 1.1340(3) 0.0456(7) Uani 1 1 d . . .
H17 H 0.3570 -0.1616 1.1291 0.055 Uiso 1 1 calc R . .
C16 C 0.5796(4) -0.0529(3) 1.2294(2) 0.0400(6) Uani 1 1 d . . .
C19 C 0.5660(5) -0.1763(3) 0.9237(3) 0.0544(8) Uani 1 1 d . . .
H19A H 0.6780 -0.1581 0.8840 0.082 Uiso 1 1 calc R . .
H19B H 0.4808 -0.1441 0.8879 0.082 Uiso 1 1 calc R . .
H19C H 0.5161 -0.2636 0.9204 0.082 Uiso 1 1 calc R . .
C13 C 1.0128(4) -0.0340(3) 1.3097(2) 0.0387(6) Uani 1 1 d . . .
H13A H 1.0426 -0.0830 1.2431 0.046 Uiso 1 1 calc R . .
H13B H 1.1251 0.0122 1.3523 0.046 Uiso 1 1 calc R . .
C18 C 0.6019(4) -0.1187(3) 1.0458(3) 0.0392(6) Uani 1 1 d . . .
N1 N 0.7551(3) -0.0118(2) 1.19931(18) 0.0340(5) Uani 1 1 d . . .
N2 N 0.7703(3) -0.0529(2) 1.08630(19) 0.0341(5) Uani 1 1 d . . .
C14 C 0.9161(4) 0.0525(3) 1.2723(2) 0.0367(6) Uani 1 1 d . . .
H14A H 0.8807 0.0974 1.3396 0.044 Uiso 1 1 calc R . .
H14B H 0.9993 0.1116 1.2309 0.044 Uiso 1 1 calc R . .
Pd1 Pd 1.0000 0.0000 1.0000 0.02952(15) Uani 1 2 d S . .
Cl1 Cl 0.97163(11) 0.19453(6) 1.01672(7) 0.0471(2) 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'
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
C8 C9 C10 120.7(4) . . ?
C9 C10 C11 119.5(4) . . ?
C9 C8 C7 120.2(4) . . ?
C12 C11 C10 120.3(4) . . ?
C4 C3 C2 119.7(5) . . ?
C5 C4 C3 121.1(4) . . ?
C1 C2 C3 119.4(5) . . ?
C12 C7 C8 119.0(3) . . ?
C12 C7 P1 122.3(3) . . ?
C8 C7 P1 118.6(3) . . ?
C11 C12 C7 120.3(4) . . ?
C4 C5 C6 120.2(4) . . ?
C6 C1 C2 120.5(3) . . ?
C6 C1 P1 121.1(3) . . ?
C2 C1 P1 118.3(3) . . ?
C1 C6 C5 119.1(4) . . ?
O1 P1 O2 115.72(15) . . ?
O1 P1 C7 113.84(18) . . ?
O2 P1 C7 100.56(15) . . ?
O1 P1 C1 112.64(16) . . ?
O2 P1 C1 105.95(13) . . ?
C7 P1 C1 107.03(15) . . ?
C13 O2 P1 119.7(2) . . ?
C16 C17 C18 107.1(3) . . ?
N1 C16 C17 107.1(3) . . ?
N1 C16 C15 121.9(3) . . ?
C17 C16 C15 130.9(3) . . ?
O2 C13 C14 108.2(2) . . ?
N2 C18 C17 109.1(3) . . ?
N2 C18 C19 121.5(3) . . ?
C17 C18 C19 129.4(3) . . ?
C16 N1 N2 110.0(2) . . ?
C16 N1 C14 128.7(2) . . ?
N2 N1 C14 120.8(2) . . ?
C18 N2 N1 106.6(2) . . ?
C18 N2 Pd1 129.0(2) . . ?
N1 N2 Pd1 123.83(18) . . ?
N1 C14 C13 112.1(2) . . ?
N2 Pd1 N2 180.00(8) . 2_757 ?
N2 Pd1 Cl1 90.58(10) . 2_757 ?
N2 Pd1 Cl1 89.42(10) 2_757 2_757 ?
N2 Pd1 Cl1 89.42(10) . . ?
N2 Pd1 Cl1 90.58(10) 2_757 . ?
Cl1 Pd1 Cl1 180.00(4) 2_757 . ?
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
C9 C8 1.366(5) . ?
C9 C10 1.386(7) . ?
C10 C11 1.377(6) . ?
C8 C7 1.393(4) . ?
C11 C12 1.376(5) . ?
C3 C4 1.366(8) . ?
C3 C2 1.396(6) . ?
C4 C5 1.352(7) . ?
C2 C1 1.383(5) . ?
C7 C12 1.391(5) . ?
C7 P1 1.791(4) . ?
C5 C6 1.404(5) . ?
C1 C6 1.374(5) . ?
C1 P1 1.797(3) . ?
O1 P1 1.470(3) . ?
P1 O2 1.591(2) . ?
O2 C13 1.454(3) . ?
C15 C16 1.497(4) . ?
C17 C16 1.366(5) . ?
C17 C18 1.387(4) . ?
C16 N1 1.355(4) . ?
C19 C18 1.491(4) . ?
C13 C14 1.508(4) . ?
C18 N2 1.343(4) . ?
N1 N2 1.368(3) . ?
N1 C14 1.453(4) . ?
N2 Pd1 2.011(4) . ?
Pd1 N2 2.011(4) 2_757 ?
Pd1 Cl1 2.2904(9) 2_757 ?
Pd1 Cl1 2.2904(9) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11 O1 0.930(4) 2.587(63) 3.411(77) 147.95(5) 3_655
