#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003390.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_7003390
loop_
_publ_author_name
'Jones, Cameron'
'Mills, David P.'
'Rose, Richard P.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis and structural characterisation of group 10 metal(ii) gallyl
 complexes: analogies with platinum diboration catalysts?
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4395
_journal_page_last               4408
_journal_paper_doi               10.1039/b715895e
_journal_year                    2008
_chemical_formula_sum            'C64 H102 Ga2 N4 P2 Pd'
_chemical_formula_weight         1235.28
_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                101.17(3)
_cell_angle_beta                 103.06(3)
_cell_angle_gamma                113.84(3)
_cell_formula_units_Z            1
_cell_length_a                   10.783(2)
_cell_length_b                   12.571(3)
_cell_length_c                   13.913(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1592.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0919
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10379
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0111P)²+1.8925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                4044
_reflns_number_total             5553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715895e.txt
_cod_data_source_block           compound8
_cod_original_cell_volume        1592.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003390
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 0.5000 0.5000 0.5000 0.01731(14) Uani 1 2 d S . .
Ga1 Ga 0.56857(4) 0.52095(4) 0.68573(3) 0.01829(14) Uani 1 1 d . . .
P1 P 0.40137(11) 0.63053(10) 0.52582(9) 0.0207(3) Uani 1 1 d . . .
N1 N 0.6704(3) 0.6549(3) 0.8122(3) 0.0195(8) Uani 1 1 d . . .
N2 N 0.5281(3) 0.4176(3) 0.7703(3) 0.0211(8) Uani 1 1 d . . .
C1 C 0.6618(4) 0.6106(4) 0.8971(3) 0.0250(10) Uani 1 1 d . . .
H1 H 0.7056 0.6646 0.9667 0.030 Uiso 1 1 calc R . .
C2 C 0.5896(4) 0.4894(4) 0.8755(3) 0.0259(11) Uani 1 1 d . . .
H2 H 0.5801 0.4533 0.9291 0.031 Uiso 1 1 calc R . .
C3 C 0.7553(4) 0.7847(4) 0.8349(3) 0.0196(10) Uani 1 1 d . . .
C4 C 0.7172(4) 0.8681(4) 0.8878(3) 0.0232(10) Uani 1 1 d . . .
C5 C 0.8051(5) 0.9938(4) 0.9095(3) 0.0298(11) Uani 1 1 d . . .
H5 H 0.7819 1.0511 0.9461 0.036 Uiso 1 1 calc R . .
C6 C 0.9238(5) 1.0361(4) 0.8792(3) 0.0306(11) Uani 1 1 d . . .
H6 H 0.9820 1.1218 0.8951 0.037 Uiso 1 1 calc R . .
C7 C 0.9589(4) 0.9539(4) 0.8255(3) 0.0263(11) Uani 1 1 d . . .
H7 H 1.0393 0.9840 0.8026 0.032 Uiso 1 1 calc R . .
C8 C 0.8788(4) 0.8280(4) 0.8044(3) 0.0219(10) Uani 1 1 d . . .
C9 C 0.5884(4) 0.8282(4) 0.9247(3) 0.0262(11) Uani 1 1 d . . .
H9 H 0.5298 0.7370 0.8937 0.031 Uiso 1 1 calc R . .
C10 C 0.6351(5) 0.8607(4) 1.0433(3) 0.0360(12) Uani 1 1 d . . .
H10A H 0.6957 0.8235 1.0664 0.054 Uiso 1 1 calc R . .
H10B H 0.5496 0.8294 1.0642 0.054 Uiso 1 1 calc R . .
H10C H 0.6899 0.9501 1.0754 0.054 Uiso 1 1 calc R . .
C11 C 0.4918(5) 0.8850(4) 0.8906(4) 0.0362(12) Uani 1 1 d . . .
H11A H 0.5424 0.9734 0.9281 0.054 Uiso 1 1 calc R . .
H11B H 0.4029 0.8467 0.9063 0.054 Uiso 1 1 calc R . .
H11C H 0.4679 0.8715 0.8155 0.054 Uiso 1 1 calc R . .
C12 C 0.9237(4) 0.7392(4) 0.7517(3) 0.0264(11) Uani 1 1 d . . .
H12 H 0.8347 0.6677 0.6986 0.032 Uiso 1 1 calc R . .
C13 C 0.9892(5) 0.6905(5) 0.8310(4) 0.0398(13) Uani 1 1 d . . .
H13A H 1.0778 0.7585 0.8836 0.060 Uiso 1 1 calc R . .
H13B H 1.0116 0.6290 0.7952 0.060 Uiso 1 1 calc R . .
H13C H 0.9201 0.6530 0.8649 0.060 Uiso 1 1 calc R . .
C14 C 1.0290(5) 0.7922(4) 0.6957(4) 0.0446(14) Uani 1 1 d . . .
H14A H 0.9885 0.8251 0.6460 0.067 Uiso 1 1 calc R . .
H14B H 1.0455 0.7274 0.6584 0.067 Uiso 1 1 calc R . .
H14C H 1.1206 0.8582 0.7468 0.067 Uiso 1 1 calc R . .
C15 C 0.4783(4) 0.2883(4) 0.7464(3) 0.0212(10) Uani 1 1 d . . .
C16 C 0.3299(4) 0.2075(4) 0.6935(3) 0.0222(10) Uani 1 1 d . . .
C17 C 0.2836(5) 0.0816(4) 0.6648(4) 0.0305(11) Uani 1 1 d . . .
H17 H 0.1846 0.0264 0.6273 0.037 Uiso 1 1 calc R . .
C18 C 0.3789(5) 0.0353(4) 0.6897(4) 0.0329(12) Uani 1 1 d . . .
H18 H 0.3451 -0.0509 0.6701 0.040 Uiso 1 1 calc R . .
C19 C 0.5232(5) 0.1149(4) 0.7431(4) 0.0340(12) Uani 1 1 d . . .
H19 H 0.5881 0.0826 0.7599 0.041 Uiso 1 1 calc R . .
C20 C 0.5756(4) 0.2422(4) 0.7731(3) 0.0267(11) Uani 1 1 d . . .
C21 C 0.2230(4) 0.2567(4) 0.6706(3) 0.0269(11) Uani 1 1 d . . .
H21 H 0.2652 0.3253 0.6424 0.032 Uiso 1 1 calc R . .
C22 C 0.2030(5) 0.3107(5) 0.7711(4) 0.0443(14) Uani 1 1 d . . .
H22A H 0.1601 0.2453 0.8003 0.066 Uiso 1 1 calc R . .
H22B H 0.1393 0.3475 0.7558 0.066 Uiso 1 1 calc R . .
H22C H 0.2969 0.3737 0.8216 0.066 Uiso 1 1 calc R . .
C23 C 0.0767(5) 0.1634(5) 0.5905(4) 0.0515(15) Uani 1 1 d . . .
H23A H 0.0898 0.1251 0.5278 0.077 Uiso 1 1 calc R . .
H23B H 0.0190 0.2048 0.5724 0.077 Uiso 1 1 calc R . .
H23C H 0.0269 0.1003 0.6196 0.077 Uiso 1 1 calc R . .
C24 C 0.7362(5) 0.3263(5) 0.8330(4) 0.0403(13) Uani 1 1 d . . .
H24 H 0.7585 0.4111 0.8316 0.048 Uiso 1 1 calc R . .
C25 C 0.7739(5) 0.3303(5) 0.9473(4) 0.0532(16) Uani 1 1 d . . .
H25A H 0.7194 0.3622 0.9804 0.080 Uiso 1 1 calc R . .
H25B H 0.8774 0.3840 0.9837 0.080 Uiso 1 1 calc R . .
H25C H 0.7491 0.2473 0.9506 0.080 Uiso 1 1 calc R . .
C26 C 0.8312(6) 0.2876(6) 0.7840(6) 0.069(2) Uani 1 1 d . . .
H26A H 0.8214 0.2097 0.7933 0.104 Uiso 1 1 calc R . .
H26B H 0.9320 0.3509 0.8176 0.104 Uiso 1 1 calc R . .
H26C H 0.8010 0.2776 0.7094 0.104 Uiso 1 1 calc R . .
C27 C 0.3814(5) 0.6806(4) 0.6507(3) 0.0284(11) Uani 1 1 d . . .
H27A H 0.4780 0.7231 0.7050 0.034 Uiso 1 1 calc R . .
H27B H 0.3456 0.7415 0.6481 0.034 Uiso 1 1 calc R . .
C28 C 0.2814(5) 0.5806(4) 0.6841(4) 0.0411(13) Uani 1 1 d . . .
H28A H 0.1900 0.5286 0.6265 0.062 Uiso 1 1 calc R . .
H28B H 0.2632 0.6183 0.7443 0.062 Uiso 1 1 calc R . .
H28C H 0.3266 0.5304 0.7031 0.062 Uiso 1 1 calc R . .
C29 C 0.5032(5) 0.7777(4) 0.5102(4) 0.0306(11) Uani 1 1 d . . .
H29A H 0.4971 0.7642 0.4364 0.037 Uiso 1 1 calc R . .
H29B H 0.4576 0.8301 0.5262 0.037 Uiso 1 1 calc R . .
C30 C 0.6604(5) 0.8457(4) 0.5780(4) 0.0447(14) Uani 1 1 d . . .
H30A H 0.6680 0.8624 0.6514 0.067 Uiso 1 1 calc R . .
H30B H 0.7077 0.9234 0.5645 0.067 Uiso 1 1 calc R . .
H30C H 0.7073 0.7954 0.5619 0.067 Uiso 1 1 calc R . .
C31 C 0.2191(4) 0.5717(4) 0.4336(4) 0.0332(12) Uani 1 1 d . . .
H31A H 0.2254 0.5682 0.3633 0.040 Uiso 1 1 calc R . .
H31B H 0.1600 0.4866 0.4316 0.040 Uiso 1 1 calc R . .
C32 C 0.1396(5) 0.6463(5) 0.4574(4) 0.0477(15) Uani 1 1 d . . .
H32A H 0.1120 0.6348 0.5185 0.072 Uiso 1 1 calc R . .
H32B H 0.0529 0.6180 0.3974 0.072 Uiso 1 1 calc R . .
H32C H 0.2033 0.7335 0.4713 0.072 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'
Ga Ga 0.2307 1.6083 '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'
P P 0.1023 0.0942 '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 P1 180.000(1) 2_666 . ?
P1 Pd1 Ga1 89.17(4) 2_666 . ?
P1 Pd1 Ga1 90.83(4) . . ?
P1 Pd1 Ga1 90.83(4) 2_666 2_666 ?
P1 Pd1 Ga1 89.17(4) . 2_666 ?
Ga1 Pd1 Ga1 180.0 . 2_666 ?
N1 Ga1 N2 86.57(14) . . ?
N1 Ga1 Pd1 135.27(10) . . ?
N2 Ga1 Pd1 137.79(10) . . ?
C29 P1 C27 100.6(2) . . ?
C29 P1 C31 103.9(2) . . ?
C27 P1 C31 102.4(2) . . ?
C29 P1 Pd1 113.30(15) . . ?
C27 P1 Pd1 120.63(15) . . ?
C31 P1 Pd1 113.89(15) . . ?
C1 N1 C3 117.4(3) . . ?
C1 N1 Ga1 109.6(3) . . ?
C3 N1 Ga1 132.9(3) . . ?
C2 N2 C15 117.7(3) . . ?
C2 N2 Ga1 109.7(3) . . ?
C15 N2 Ga1 130.9(3) . . ?
C2 C1 N1 117.0(4) . . ?
C1 C2 N2 117.1(4) . . ?
C4 C3 C8 120.4(4) . . ?
C4 C3 N1 120.5(4) . . ?
C8 C3 N1 119.1(4) . . ?
C5 C4 C3 118.2(4) . . ?
C5 C4 C9 118.6(4) . . ?
C3 C4 C9 123.2(4) . . ?
C6 C5 C4 121.6(4) . . ?
C5 C6 C7 120.0(4) . . ?
C6 C7 C8 121.3(4) . . ?
C7 C8 C3 118.4(4) . . ?
C7 C8 C12 121.0(4) . . ?
C3 C8 C12 120.6(4) . . ?
C4 C9 C11 112.6(4) . . ?
C4 C9 C10 111.6(4) . . ?
C11 C9 C10 108.4(4) . . ?
C8 C12 C14 114.5(4) . . ?
C8 C12 C13 110.2(4) . . ?
C14 C12 C13 109.2(4) . . ?
C20 C15 C16 120.5(4) . . ?
C20 C15 N2 120.6(4) . . ?
C16 C15 N2 118.9(4) . . ?
C17 C16 C15 118.6(4) . . ?
C17 C16 C21 120.7(4) . . ?
C15 C16 C21 120.7(4) . . ?
C18 C17 C16 121.3(4) . . ?
C19 C18 C17 119.7(4) . . ?
C18 C19 C20 121.3(4) . . ?
C19 C20 C15 118.6(4) . . ?
C19 C20 C24 119.2(4) . . ?
C15 C20 C24 122.3(4) . . ?
C16 C21 C23 114.4(4) . . ?
C16 C21 C22 110.5(4) . . ?
C23 C21 C22 109.4(4) . . ?
C20 C24 C26 112.2(5) . . ?
C20 C24 C25 111.0(4) . . ?
C26 C24 C25 109.5(4) . . ?
C28 C27 P1 116.3(3) . . ?
C30 C29 P1 114.5(3) . . ?
C32 C31 P1 115.9(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 P1 2.3038(12) 2_666 ?
Pd1 P1 2.3038(12) . ?
Pd1 Ga1 2.4514(8) . ?
Pd1 Ga1 2.4514(8) 2_666 ?
Ga1 N1 1.903(3) . ?
Ga1 N2 1.905(3) . ?
P1 C29 1.816(5) . ?
P1 C27 1.820(5) . ?
P1 C31 1.837(4) . ?
N1 C1 1.406(5) . ?
N1 C3 1.436(5) . ?
N2 C2 1.401(5) . ?
N2 C15 1.430(5) . ?
C1 C2 1.332(6) . ?
C3 C4 1.414(6) . ?
C3 C8 1.417(6) . ?
C4 C5 1.400(6) . ?
C4 C9 1.517(6) . ?
C5 C6 1.371(6) . ?
C6 C7 1.383(6) . ?
C7 C8 1.392(6) . ?
C8 C12 1.515(6) . ?
C9 C11 1.526(6) . ?
C9 C10 1.531(6) . ?
C12 C14 1.527(6) . ?
C12 C13 1.533(6) . ?
C15 C20 1.405(6) . ?
C15 C16 1.414(6) . ?
C16 C17 1.392(6) . ?
C16 C21 1.517(6) . ?
C17 C18 1.384(6) . ?
C18 C19 1.380(6) . ?
C19 C20 1.400(6) . ?
C20 C24 1.529(6) . ?
C21 C23 1.520(6) . ?
C21 C22 1.533(6) . ?
C24 C26 1.530(7) . ?
C24 C25 1.534(7) . ?
C27 C28 1.522(6) . ?
C29 C30 1.512(6) . ?
C31 C32 1.543(6) . ?
