#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003388.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_7003388
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 Pt'
_chemical_formula_weight         1323.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 109.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.646(3)
_cell_length_b                   19.976(4)
_cell_length_c                   21.147(4)
_cell_measurement_temperature    150(2)
_cell_volume                     6239(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10556
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.780
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0459
_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)+(0.0221P)²+44.4146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                4639
_reflns_number_total             5450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715895e.txt
_cod_data_source_block           compound6
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7003388
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Pt1 Pt 0.5000 0.480507(15) 0.7500 0.02359(10) Uani 1 2 d S . .
Ga1 Ga 0.40229(4) 0.38415(3) 0.74278(3) 0.02350(16) Uani 1 1 d . . .
P1 P 0.61713(10) 0.55295(8) 0.75341(8) 0.0316(4) Uani 1 1 d . . .
N1 N 0.3080(3) 0.3552(2) 0.6646(2) 0.0264(10) Uani 1 1 d . . .
N2 N 0.3807(3) 0.3063(2) 0.7871(2) 0.0250(10) Uani 1 1 d . . .
C1 C 0.2751(4) 0.2935(3) 0.6784(3) 0.0277(13) Uani 1 1 d . . .
H1 H 0.2284 0.2702 0.6453 0.033 Uiso 1 1 calc R . .
C2 C 0.3122(4) 0.2691(3) 0.7402(3) 0.0280(13) Uani 1 1 d . . .
H2 H 0.2929 0.2274 0.7523 0.034 Uiso 1 1 calc R . .
C3 C 0.2550(3) 0.3932(3) 0.6085(3) 0.0254(12) Uani 1 1 d . . .
C4 C 0.1655(4) 0.4131(3) 0.6031(3) 0.0296(13) Uani 1 1 d . . .
C5 C 0.1159(4) 0.4509(3) 0.5486(3) 0.0381(15) Uani 1 1 d . . .
H5 H 0.0552 0.4625 0.5440 0.046 Uiso 1 1 calc R . .
C6 C 0.1520(4) 0.4721(3) 0.5008(3) 0.0409(16) Uani 1 1 d . . .
H6 H 0.1175 0.4993 0.4645 0.049 Uiso 1 1 calc R . .
C7 C 0.2395(4) 0.4532(3) 0.5065(3) 0.0351(14) Uani 1 1 d . . .
H7 H 0.2645 0.4680 0.4736 0.042 Uiso 1 1 calc R . .
C8 C 0.2914(4) 0.4134(3) 0.5587(3) 0.0291(13) Uani 1 1 d . . .
C9 C 0.1232(4) 0.3961(3) 0.6563(3) 0.0324(14) Uani 1 1 d . . .
H9 H 0.1717 0.3772 0.6958 0.039 Uiso 1 1 calc R . .
C10 C 0.0497(4) 0.3431(3) 0.6312(3) 0.0426(16) Uani 1 1 d . . .
H10A H 0.0277 0.3300 0.6678 0.064 Uiso 1 1 calc R . .
H10B H 0.0747 0.3038 0.6158 0.064 Uiso 1 1 calc R . .
H10C H -0.0006 0.3614 0.5941 0.064 Uiso 1 1 calc R . .
C11 C 0.0836(4) 0.4575(3) 0.6798(3) 0.0441(17) Uani 1 1 d . . .
H11A H 0.0282 0.4715 0.6446 0.066 Uiso 1 1 calc R . .
H11B H 0.1279 0.4940 0.6896 0.066 Uiso 1 1 calc R . .
H11C H 0.0695 0.4462 0.7204 0.066 Uiso 1 1 calc R . .
C12 C 0.3853(4) 0.3926(3) 0.5596(3) 0.0310(14) Uani 1 1 d . . .
H12 H 0.4098 0.3590 0.5961 0.037 Uiso 1 1 calc R . .
C13 C 0.3819(5) 0.3604(4) 0.4931(3) 0.0497(18) Uani 1 1 d . . .
H13A H 0.3382 0.3234 0.4827 0.075 Uiso 1 1 calc R . .
H13B H 0.4420 0.3432 0.4967 0.075 Uiso 1 1 calc R . .
H13C H 0.3632 0.3939 0.4573 0.075 Uiso 1 1 calc R . .
C14 C 0.4505(4) 0.4520(3) 0.5733(3) 0.0441(16) Uani 1 1 d . . .
H14A H 0.4284 0.4851 0.5373 0.066 Uiso 1 1 calc R . .
H14B H 0.5107 0.4365 0.5751 0.066 Uiso 1 1 calc R . .
H14C H 0.4542 0.4726 0.6161 0.066 Uiso 1 1 calc R . .
C15 C 0.3935(4) 0.2878(3) 0.8561(3) 0.0272(13) Uani 1 1 d . . .
C16 C 0.3296(4) 0.3108(3) 0.8861(3) 0.0280(13) Uani 1 1 d . . .
C17 C 0.3387(4) 0.2896(3) 0.9504(3) 0.0362(15) Uani 1 1 d . . .
H17 H 0.2973 0.3055 0.9712 0.043 Uiso 1 1 calc R . .
C18 C 0.4063(4) 0.2459(3) 0.9849(3) 0.0381(15) Uani 1 1 d . . .
H18 H 0.4111 0.2317 1.0288 0.046 Uiso 1 1 calc R . .
C19 C 0.4666(4) 0.2233(3) 0.9551(3) 0.0360(15) Uani 1 1 d . . .
H19 H 0.5130 0.1931 0.9789 0.043 Uiso 1 1 calc R . .
C20 C 0.4618(4) 0.2432(3) 0.8910(3) 0.0312(14) Uani 1 1 d . . .
C21 C 0.2490(4) 0.3547(3) 0.8491(3) 0.0346(14) Uani 1 1 d . . .
H21 H 0.2608 0.3742 0.8092 0.042 Uiso 1 1 calc R . .
C22 C 0.1629(4) 0.3128(3) 0.8238(3) 0.0435(17) Uani 1 1 d . . .
H22A H 0.1715 0.2769 0.7950 0.065 Uiso 1 1 calc R . .
H22B H 0.1123 0.3413 0.7982 0.065 Uiso 1 1 calc R . .
H22C H 0.1496 0.2933 0.8621 0.065 Uiso 1 1 calc R . .
C23 C 0.2363(5) 0.4125(3) 0.8921(4) 0.0493(18) Uani 1 1 d . . .
H23A H 0.2190 0.3948 0.9294 0.074 Uiso 1 1 calc R . .
H23B H 0.1887 0.4424 0.8648 0.074 Uiso 1 1 calc R . .
H23C H 0.2932 0.4375 0.9099 0.074 Uiso 1 1 calc R . .
C24 C 0.5275(4) 0.2115(3) 0.8596(3) 0.0382(15) Uani 1 1 d . . .
H24 H 0.5302 0.2407 0.8219 0.046 Uiso 1 1 calc R . .
C25 C 0.6231(4) 0.2027(3) 0.9081(3) 0.0422(16) Uani 1 1 d . . .
H25A H 0.6218 0.1735 0.9451 0.063 Uiso 1 1 calc R . .
H25B H 0.6479 0.2464 0.9259 0.063 Uiso 1 1 calc R . .
H25C H 0.6611 0.1824 0.8846 0.063 Uiso 1 1 calc R . .
C26 C 0.4907(5) 0.1435(4) 0.8312(4) 0.066(2) Uani 1 1 d . . .
H26A H 0.5336 0.1217 0.8130 0.099 Uiso 1 1 calc R . .
H26B H 0.4324 0.1494 0.7955 0.099 Uiso 1 1 calc R . .
H26C H 0.4823 0.1157 0.8668 0.099 Uiso 1 1 calc R . .
C27 C 0.5929(4) 0.6394(3) 0.7260(3) 0.0419(16) Uani 1 1 d . . .
H27A H 0.5661 0.6627 0.7564 0.050 Uiso 1 1 calc R . .
H27B H 0.6503 0.6623 0.7293 0.050 Uiso 1 1 calc R . .
C28 C 0.5277(5) 0.6449(4) 0.6539(3) 0.0512(18) Uani 1 1 d . . .
H28A H 0.5549 0.6237 0.6234 0.077 Uiso 1 1 calc R . .
H28B H 0.5158 0.6922 0.6419 0.077 Uiso 1 1 calc R . .
H28C H 0.4706 0.6224 0.6504 0.077 Uiso 1 1 calc R . .
C29 C 0.6839(4) 0.5261(3) 0.7015(3) 0.0404(15) Uani 1 1 d . . .
H29A H 0.7158 0.4843 0.7210 0.048 Uiso 1 1 calc R . .
H29B H 0.6412 0.5148 0.6566 0.048 Uiso 1 1 calc R . .
C30 C 0.7546(4) 0.5750(3) 0.6918(3) 0.0429(16) Uani 1 1 d . . .
H30A H 0.7243 0.6159 0.6702 0.064 Uiso 1 1 calc R . .
H30B H 0.7857 0.5540 0.6636 0.064 Uiso 1 1 calc R . .
H30C H 0.7989 0.5861 0.7355 0.064 Uiso 1 1 calc R . .
C31 C 0.6992(4) 0.5609(3) 0.8397(4) 0.0487(18) Uani 1 1 d . . .
H31A H 0.6656 0.5503 0.8707 0.058 Uiso 1 1 calc R . .
H31B H 0.7445 0.5248 0.8450 0.058 Uiso 1 1 calc R . .
C32 C 0.7498(7) 0.6220(4) 0.8644(5) 0.092(3) Uani 1 1 d . . .
H32A H 0.7894 0.6318 0.8380 0.138 Uiso 1 1 calc R . .
H32B H 0.7866 0.6162 0.9116 0.138 Uiso 1 1 calc R . .
H32C H 0.7075 0.6593 0.8603 0.138 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'
P P 0.1023 0.0942 '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'
Pt Pt -1.7033 8.3905 '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 Pt1 P1 102.71(8) . 2_656 ?
P1 Pt1 Ga1 166.10(4) . . ?
P1 Pt1 Ga1 91.04(4) 2_656 . ?
P1 Pt1 Ga1 91.04(4) . 2_656 ?
P1 Pt1 Ga1 166.10(4) 2_656 2_656 ?
Ga1 Pt1 Ga1 75.31(3) . 2_656 ?
N2 Ga1 N1 88.03(19) . . ?
N2 Ga1 Pt1 145.77(14) . . ?
N1 Ga1 Pt1 125.84(14) . . ?
C27 P1 C29 100.8(3) . . ?
C27 P1 C31 103.6(3) . . ?
C29 P1 C31 105.5(3) . . ?
C27 P1 Pt1 120.2(2) . . ?
C29 P1 Pt1 113.6(2) . . ?
C31 P1 Pt1 111.5(2) . . ?
C1 N1 C3 119.3(4) . . ?
C1 N1 Ga1 108.6(4) . . ?
C3 N1 Ga1 129.2(4) . . ?
C2 N2 C15 113.3(4) . . ?
C2 N2 Ga1 107.6(3) . . ?
C15 N2 Ga1 135.5(4) . . ?
C2 C1 N1 116.9(5) . . ?
C1 C2 N2 118.8(5) . . ?
C8 C3 C4 119.3(5) . . ?
C8 C3 N1 120.5(5) . . ?
C4 C3 N1 120.2(5) . . ?
C5 C4 C3 119.2(5) . . ?
C5 C4 C9 118.4(5) . . ?
C3 C4 C9 122.4(5) . . ?
C6 C5 C4 121.7(5) . . ?
C5 C6 C7 119.0(6) . . ?
C8 C7 C6 121.9(6) . . ?
C7 C8 C3 118.9(5) . . ?
C7 C8 C12 118.5(5) . . ?
C3 C8 C12 122.6(5) . . ?
C4 C9 C10 111.2(5) . . ?
C4 C9 C11 112.5(5) . . ?
C10 C9 C11 109.3(5) . . ?
C8 C12 C14 111.8(5) . . ?
C8 C12 C13 111.2(5) . . ?
C14 C12 C13 108.7(5) . . ?
C20 C15 C16 119.6(5) . . ?
C20 C15 N2 121.3(5) . . ?
C16 C15 N2 118.8(5) . . ?
C17 C16 C15 118.6(5) . . ?
C17 C16 C21 118.7(5) . . ?
C15 C16 C21 122.6(5) . . ?
C18 C17 C16 121.6(6) . . ?
C19 C18 C17 119.3(6) . . ?
C18 C19 C20 121.9(6) . . ?
C19 C20 C15 118.9(5) . . ?
C19 C20 C24 118.4(5) . . ?
C15 C20 C24 122.6(5) . . ?
C23 C21 C16 112.2(5) . . ?
C23 C21 C22 110.6(5) . . ?
C16 C21 C22 110.4(5) . . ?
C25 C24 C26 108.9(5) . . ?
C25 C24 C20 114.0(5) . . ?
C26 C24 C20 108.7(5) . . ?
C28 C27 P1 112.6(5) . . ?
C30 C29 P1 118.2(4) . . ?
C32 C31 P1 122.8(6) . . ?
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
Pt1 P1 2.3173(15) . ?
Pt1 P1 2.3173(15) 2_656 ?
Pt1 Ga1 2.4313(7) . ?
Pt1 Ga1 2.4313(7) 2_656 ?
Ga1 N2 1.903(4) . ?
Ga1 N1 1.906(4) . ?
P1 C27 1.822(6) . ?
P1 C29 1.829(6) . ?
P1 C31 1.859(7) . ?
N1 C1 1.402(7) . ?
N1 C3 1.423(7) . ?
N2 C2 1.406(7) . ?
N2 C15 1.453(7) . ?
C1 C2 1.333(8) . ?
C3 C8 1.412(8) . ?
C3 C4 1.423(7) . ?
C4 C5 1.381(8) . ?
C4 C9 1.521(8) . ?
C5 C6 1.378(9) . ?
C6 C7 1.386(8) . ?
C7 C8 1.386(8) . ?
C8 C12 1.520(8) . ?
C9 C10 1.523(8) . ?
C9 C11 1.529(8) . ?
C12 C14 1.528(8) . ?
C12 C13 1.531(8) . ?
C15 C20 1.401(8) . ?
C15 C16 1.426(8) . ?
C16 C17 1.385(8) . ?
C16 C21 1.523(8) . ?
C17 C18 1.380(8) . ?
C18 C19 1.373(8) . ?
C19 C20 1.390(8) . ?
C20 C24 1.533(8) . ?
C21 C23 1.522(8) . ?
C21 C22 1.526(9) . ?
C24 C25 1.518(8) . ?
C24 C26 1.519(9) . ?
C27 C28 1.533(9) . ?
C29 C30 1.539(8) . ?
C31 C32 1.455(10) . ?
