#------------------------------------------------------------------------------
#$Date: 2016-02-05 01:50:43 +0200 (Fri, 05 Feb 2016) $
#$Revision: 176063 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/74/7037448.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_7037448
loop_
_publ_author_name
'Adam, Mohamed Shaker S.'
'Kindermann, Markus K.'
'Jones, Peter G.'
'Heinicke, Joachim W.'
_publ_section_title
;
 3H-1,3-Azaphospholo[4,5-b]pyridines - novel heterocyclic P,N-bridging or
 hybrid ligands: synthesis and first d(8)-transition metal complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2261
_journal_page_last               2272
_journal_paper_doi               10.1039/c5dt04073f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C36 H54 Cl10 N4 P2 Pd3'
_chemical_formula_weight         1278.47
_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
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                101.959(4)
_cell_angle_beta                 92.199(4)
_cell_angle_gamma                109.528(4)
_cell_formula_units_Z            1
_cell_length_a                   8.5594(7)
_cell_length_b                   9.6780(8)
_cell_length_c                   16.4206(13)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.3
_cell_volume                     1245.60(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2 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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38910
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_correction_T_min  0.8080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.527
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         7630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0248
_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)+(0.0232P)²+1.7489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                6560
_reflns_number_total             7630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04073f3.cif
_cod_data_source_block           effri
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037445--7037448.cif.
;
_cod_database_code               7037448
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
Pd1 Pd 0.566573(18) 0.140529(16) 0.856527(9) 0.01373(4) Uani 1 1 d .
Cl1 Cl 0.27524(6) 0.03495(6) 0.85481(3) 0.02193(10) Uani 1 1 d .
Pd2 Pd 0.5000 0.5000 1.0000 0.01116(4) Uani 1 2 d S
Cl2 Cl 0.65679(6) 0.37760(6) 1.05057(3) 0.01936(9) Uani 1 1 d .
N1 N 0.80247(19) 0.48648(18) 0.72467(10) 0.0131(3) Uani 1 1 d .
C2 C 0.6767(2) 0.3622(2) 0.70925(11) 0.0124(3) Uani 1 1 d .
P3 P 0.55508(6) 0.33098(5) 0.79874(3) 0.01095(9) Uani 1 1 d .
C3A C 0.6906(2) 0.51571(19) 0.85546(11) 0.0110(3) Uani 1 1 d .
N4 N 0.68534(19) 0.58801(17) 0.93353(10) 0.0121(3) Uani 1 1 d .
C5 C 0.8066(2) 0.7217(2) 0.96668(12) 0.0156(3) Uani 1 1 d .
H5 H 0.8029 0.7750 1.0217 0.019 Uiso 1 1 calc R
C6 C 0.9369(2) 0.7835(2) 0.92226(12) 0.0173(4) Uani 1 1 d .
H6 H 1.0221 0.8769 0.9477 0.021 Uiso 1 1 calc R
C7 C 0.9437(2) 0.7101(2) 0.84107(12) 0.0158(4) Uani 1 1 d .
H7 H 1.0322 0.7512 0.8102 0.019 Uiso 1 1 calc R
C7A C 0.8162(2) 0.5745(2) 0.80694(11) 0.0124(3) Uani 1 1 d .
C8 C 0.6447(2) 0.2448(2) 0.62727(12) 0.0152(3) Uani 1 1 d .
C9 C 0.7509(3) 0.1476(2) 0.63677(13) 0.0213(4) Uani 1 1 d .
H9A H 0.8683 0.2125 0.6522 0.032 Uiso 1 1 calc R
H9B H 0.7394 0.0749 0.5835 0.032 Uiso 1 1 calc R
H9C H 0.7128 0.0933 0.6806 0.032 Uiso 1 1 calc R
C10 C 0.6977(3) 0.3231(3) 0.55571(13) 0.0245(4) Uani 1 1 d .
H10A H 0.6316 0.3869 0.5506 0.037 Uiso 1 1 calc R
H10B H 0.6790 0.2470 0.5031 0.037 Uiso 1 1 calc R
H10C H 0.8163 0.3855 0.5675 0.037 Uiso 1 1 calc R
C11 C 0.4607(3) 0.1433(3) 0.60875(14) 0.0252(5) Uani 1 1 d .
H11A H 0.4277 0.0955 0.6555 0.038 Uiso 1 1 calc R
H11B H 0.4447 0.0653 0.5573 0.038 Uiso 1 1 calc R
H11C H 0.3920 0.2041 0.6016 0.038 Uiso 1 1 calc R
C12 C 0.3559(2) 0.3521(2) 0.77214(12) 0.0147(3) Uani 1 1 d .
H12A H 0.2814 0.2572 0.7341 0.018 Uiso 1 1 calc R
H12B H 0.3025 0.3681 0.8240 0.018 Uiso 1 1 calc R
C13 C 0.3726(2) 0.4822(2) 0.73033(13) 0.0172(4) Uani 1 1 d .
H13A H 0.4536 0.5761 0.7663 0.021 Uiso 1 1 calc R
H13B H 0.4173 0.4625 0.6761 0.021 Uiso 1 1 calc R
C14 C 0.2074(3) 0.5044(3) 0.71517(14) 0.0228(4) Uani 1 1 d .
H14A H 0.1622 0.5233 0.7693 0.027 Uiso 1 1 calc R
H14B H 0.1267 0.4109 0.6787 0.027 Uiso 1 1 calc R
C15 C 0.2256(3) 0.6353(3) 0.67424(17) 0.0330(6) Uani 1 1 d .
H15A H 0.2999 0.7291 0.7117 0.050 Uiso 1 1 calc R
H15B H 0.1158 0.6430 0.6633 0.050 Uiso 1 1 calc R
H15C H 0.2729 0.6182 0.6212 0.050 Uiso 1 1 calc R
C16 C 0.6470(3) -0.0072(3) 0.92001(18) 0.0317(5) Uani 1 1 d .
H16A H 0.582(4) -0.106(4) 0.905(2) 0.038(8) Uiso 1 1 d .
H16B H 0.662(4) 0.061(3) 0.977(2) 0.034(8) Uiso 1 1 d .
C17 C 0.7616(3) 0.0482(3) 0.86699(17) 0.0304(5) Uani 1 1 d .
H17 H 0.767(3) -0.022(3) 0.8129(18) 0.027(7) Uiso 1 1 d .
C18 C 0.8304(3) 0.2037(3) 0.87476(15) 0.0237(4) Uani 1 1 d .
H18A H 0.856(4) 0.269(3) 0.9279(19) 0.034(8) Uiso 1 1 d .
H18B H 0.896(3) 0.245(3) 0.8357(18) 0.027(7) Uiso 1 1 d .
C99 C 0.8527(3) 0.7495(3) 0.60772(15) 0.0255(4) Uani 1 1 d .
H99 H 0.8671 0.6614 0.6257 0.031 Uiso 1 1 calc R
Cl3 Cl 0.64749(7) 0.74110(7) 0.61951(5) 0.03518(14) Uani 1 1 d .
Cl4 Cl 0.99626(8) 0.91344(7) 0.67272(5) 0.03601(14) Uani 1 1 d .
Cl5 Cl 0.88653(13) 0.73198(14) 0.50305(5) 0.0679(3) 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'
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
C18 Pd1 C17 38.05(10) . .
C18 Pd1 C16 67.44(10) . .
C17 Pd1 C16 37.05(10) . .
C18 Pd1 P3 97.89(7) . .
C17 Pd1 P3 131.02(7) . .
C16 Pd1 P3 165.00(8) . .
C18 Pd1 Cl1 167.66(7) . .
C17 Pd1 Cl1 131.73(8) . .
C16 Pd1 Cl1 100.35(7) . .
P3 Pd1 Cl1 94.182(19) . .
N4 Pd2 N4 180.0 2_667 .
N4 Pd2 Cl2 89.37(5) 2_667 2_667
N4 Pd2 Cl2 90.63(5) . 2_667
N4 Pd2 Cl2 90.63(5) 2_667 .
N4 Pd2 Cl2 89.37(5) . .
Cl2 Pd2 Cl2 180.0 2_667 .
C2 N1 C7A 112.59(16) . .
N1 C2 C8 121.76(17) . .
N1 C2 P3 114.44(14) . .
C8 C2 P3 123.46(14) . .
C3A P3 C12 105.39(9) . .
C3A P3 C2 87.36(8) . .
C12 P3 C2 106.44(9) . .
C3A P3 Pd1 114.31(6) . .
C12 P3 Pd1 121.33(6) . .
C2 P3 Pd1 116.46(6) . .
N4 C3A C7A 122.45(16) . .
N4 C3A P3 127.97(14) . .
C7A C3A P3 109.47(13) . .
C3A N4 C5 118.54(16) . .
C3A N4 Pd2 120.86(12) . .
C5 N4 Pd2 120.59(13) . .
N4 C5 C6 121.50(17) . .
C7 C6 C5 120.60(18) . .
C7A C7 C6 117.37(17) . .
C7 C7A C3A 119.50(17) . .
C7 C7A N1 124.65(17) . .
C3A C7A N1 115.85(16) . .
C2 C8 C10 109.74(16) . .
C2 C8 C11 111.13(16) . .
C10 C8 C11 110.25(18) . .
C2 C8 C9 107.25(16) . .
C10 C8 C9 109.57(17) . .
C11 C8 C9 108.84(17) . .
C13 C12 P3 113.70(13) . .
C14 C13 C12 112.44(16) . .
C13 C14 C15 112.05(18) . .
C17 C16 Pd1 69.92(14) . .
C16 C17 C18 119.4(2) . .
C16 C17 Pd1 73.03(14) . .
C18 C17 Pd1 69.71(13) . .
C17 C18 Pd1 72.25(14) . .
Cl5 C99 Cl4 112.42(14) . .
Cl5 C99 Cl3 110.38(13) . .
Cl4 C99 Cl3 111.01(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C18 2.125(2) .
Pd1 C17 2.157(2) .
Pd1 C16 2.197(2) .
Pd1 P3 2.2685(5) .
Pd1 Cl1 2.3542(5) .
Pd2 N4 2.0120(15) 2_667
Pd2 N4 2.0121(15) .
Pd2 Cl2 2.2976(5) 2_667
Pd2 Cl2 2.2976(5) .
N1 C2 1.288(2) .
N1 C7A 1.417(2) .
C2 C8 1.519(3) .
C2 P3 1.8506(19) .
P3 C3A 1.8027(18) .
P3 C12 1.8305(19) .
C3A N4 1.337(2) .
C3A C7A 1.400(2) .
N4 C5 1.347(2) .
C5 C6 1.390(3) .
C6 C7 1.388(3) .
C7 C7A 1.385(3) .
C8 C10 1.530(3) .
C8 C11 1.531(3) .
C8 C9 1.536(3) .
C12 C13 1.524(3) .
C13 C14 1.519(3) .
C14 C15 1.520(3) .
C16 C17 1.384(4) .
C17 C18 1.396(4) .
C99 Cl5 1.737(3) .
C99 Cl4 1.750(2) .
C99 Cl3 1.751(2) .
