#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003389.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_7003389
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 Ni P2'
_chemical_formula_weight         1187.59
_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                101.19(3)
_cell_angle_beta                 103.22(3)
_cell_angle_gamma                113.31(3)
_cell_formula_units_Z            1
_cell_length_a                   10.788(2)
_cell_length_b                   12.518(3)
_cell_length_c                   13.824(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1582.2(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11700
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0413
_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)+(0.0218P)²+0.9960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                4982
_reflns_number_total             6451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715895e.txt
_cod_data_source_block           compound7
_cod_original_cell_volume        1582.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003389
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
Ga1 Ga 0.56745(3) 0.51972(2) 0.68005(2) 0.01469(9) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.01424(12) Uani 1 2 d S . .
P1 P 0.40269(7) 0.62218(6) 0.52584(6) 0.01758(16) Uani 1 1 d . . .
N1 N 0.5248(2) 0.41563(18) 0.76477(17) 0.0180(5) Uani 1 1 d . . .
N2 N 0.6700(2) 0.65329(18) 0.80842(16) 0.0154(5) Uani 1 1 d . . .
C1 C 0.5863(3) 0.4868(2) 0.8705(2) 0.0229(6) Uani 1 1 d . . .
H1 H 0.5768 0.4503 0.9243 0.027 Uiso 1 1 calc R . .
C2 C 0.6592(3) 0.6084(2) 0.8929(2) 0.0206(6) Uani 1 1 d . . .
H2 H 0.7019 0.6619 0.9631 0.025 Uiso 1 1 calc R . .
C3 C 0.4742(3) 0.2864(2) 0.7414(2) 0.0169(6) Uani 1 1 d . . .
C4 C 0.3260(3) 0.2062(2) 0.6907(2) 0.0201(6) Uani 1 1 d . . .
C5 C 0.2791(3) 0.0800(2) 0.6639(2) 0.0261(7) Uani 1 1 d . . .
H5 H 0.1800 0.0252 0.6288 0.031 Uiso 1 1 calc R . .
C6 C 0.3756(3) 0.0336(3) 0.6880(2) 0.0301(7) Uani 1 1 d . . .
H6 H 0.3424 -0.0526 0.6682 0.036 Uiso 1 1 calc R . .
C7 C 0.5186(3) 0.1117(3) 0.7400(2) 0.0280(7) Uani 1 1 d . . .
H7 H 0.5828 0.0784 0.7575 0.034 Uiso 1 1 calc R . .
C8 C 0.5720(3) 0.2388(2) 0.7681(2) 0.0217(6) Uani 1 1 d . . .
C9 C 0.2199(3) 0.2578(2) 0.6696(2) 0.0238(6) Uani 1 1 d . . .
H9 H 0.2612 0.3267 0.6415 0.029 Uiso 1 1 calc R . .
C10 C 0.2011(4) 0.3105(3) 0.7718(3) 0.0370(8) Uani 1 1 d . . .
H10A H 0.1592 0.2445 0.8007 0.056 Uiso 1 1 calc R . .
H10B H 0.1372 0.3479 0.7577 0.056 Uiso 1 1 calc R . .
H10C H 0.2947 0.3729 0.8225 0.056 Uiso 1 1 calc R . .
C11 C 0.0736(3) 0.1643(3) 0.5890(3) 0.0435(9) Uani 1 1 d . . .
H11A H 0.0865 0.1264 0.5256 0.065 Uiso 1 1 calc R . .
H11B H 0.0152 0.2056 0.5715 0.065 Uiso 1 1 calc R . .
H11C H 0.0252 0.1008 0.6183 0.065 Uiso 1 1 calc R . .
C12 C 0.7315(3) 0.3216(3) 0.8252(3) 0.0352(8) Uani 1 1 d . . .
H12 H 0.7529 0.4061 0.8225 0.042 Uiso 1 1 calc R . .
C13 C 0.7742(4) 0.3283(3) 0.9404(3) 0.0524(10) Uani 1 1 d . . .
H13A H 0.7224 0.3625 0.9752 0.079 Uiso 1 1 calc R . .
H13B H 0.8777 0.3810 0.9746 0.079 Uiso 1 1 calc R . .
H13C H 0.7499 0.2458 0.9451 0.079 Uiso 1 1 calc R . .
C14 C 0.8232(4) 0.2803(4) 0.7738(4) 0.0603(12) Uani 1 1 d . . .
H14A H 0.8152 0.2031 0.7848 0.091 Uiso 1 1 calc R . .
H14B H 0.9237 0.3433 0.8051 0.091 Uiso 1 1 calc R . .
H14C H 0.7896 0.2679 0.6984 0.091 Uiso 1 1 calc R . .
C15 C 0.7546(3) 0.7831(2) 0.8331(2) 0.0173(6) Uani 1 1 d . . .
C16 C 0.7155(3) 0.8665(2) 0.8865(2) 0.0201(6) Uani 1 1 d . . .
C17 C 0.8026(3) 0.9919(2) 0.9091(2) 0.0259(7) Uani 1 1 d . . .
H17 H 0.7781 1.0489 0.9456 0.031 Uiso 1 1 calc R . .
C18 C 0.9216(3) 1.0354(3) 0.8805(2) 0.0293(7) Uani 1 1 d . . .
H18 H 0.9783 1.1212 0.8967 0.035 Uiso 1 1 calc R . .
C19 C 0.9590(3) 0.9533(2) 0.8277(2) 0.0260(7) Uani 1 1 d . . .
H19 H 1.0416 0.9838 0.8075 0.031 Uiso 1 1 calc R . .
C20 C 0.8779(3) 0.8269(2) 0.8036(2) 0.0196(6) Uani 1 1 d . . .
C21 C 0.5865(3) 0.8264(3) 0.9236(2) 0.0226(6) Uani 1 1 d . . .
H21 H 0.5283 0.7354 0.8919 0.027 Uiso 1 1 calc R . .
C22 C 0.6339(3) 0.8575(3) 1.0428(2) 0.0316(7) Uani 1 1 d . . .
H22A H 0.6935 0.8187 1.0651 0.047 Uiso 1 1 calc R . .
H22B H 0.5491 0.8272 1.0642 0.047 Uiso 1 1 calc R . .
H22C H 0.6894 0.9467 1.0756 0.047 Uiso 1 1 calc R . .
C23 C 0.4896(3) 0.8850(3) 0.8899(2) 0.0321(7) Uani 1 1 d . . .
H23A H 0.5406 0.9734 0.9274 0.048 Uiso 1 1 calc R . .
H23B H 0.4018 0.8478 0.9065 0.048 Uiso 1 1 calc R . .
H23C H 0.4648 0.8713 0.8142 0.048 Uiso 1 1 calc R . .
C24 C 0.9258(3) 0.7385(2) 0.7521(2) 0.0239(6) Uani 1 1 d . . .
H24 H 0.8383 0.6675 0.6976 0.029 Uiso 1 1 calc R . .
C25 C 0.9883(3) 0.6881(3) 0.8319(3) 0.0376(8) Uani 1 1 d . . .
H25A H 1.0761 0.7551 0.8856 0.056 Uiso 1 1 calc R . .
H25B H 1.0108 0.6260 0.7962 0.056 Uiso 1 1 calc R . .
H25C H 0.9181 0.6508 0.8649 0.056 Uiso 1 1 calc R . .
C26 C 1.0318(3) 0.7930(3) 0.6971(3) 0.0417(9) Uani 1 1 d . . .
H26A H 0.9913 0.8261 0.6469 0.063 Uiso 1 1 calc R . .
H26B H 1.0501 0.7288 0.6599 0.063 Uiso 1 1 calc R . .
H26C H 1.1220 0.8589 0.7492 0.063 Uiso 1 1 calc R . .
C27 C 0.3840(3) 0.6759(2) 0.6524(2) 0.0212(6) Uani 1 1 d . . .
H27A H 0.4807 0.7194 0.7065 0.025 Uiso 1 1 calc R . .
H27B H 0.3473 0.7366 0.6484 0.025 Uiso 1 1 calc R . .
C28 C 0.2866(3) 0.5785(3) 0.6888(3) 0.0324(7) Uani 1 1 d . . .
H28A H 0.1970 0.5231 0.6306 0.049 Uiso 1 1 calc R . .
H28B H 0.2654 0.6180 0.7469 0.049 Uiso 1 1 calc R . .
H28C H 0.3348 0.5315 0.7125 0.049 Uiso 1 1 calc R . .
C29 C 0.2191(3) 0.5641(3) 0.4354(2) 0.0280(7) Uani 1 1 d . . .
H29A H 0.2235 0.5603 0.3642 0.034 Uiso 1 1 calc R . .
H29B H 0.1619 0.4789 0.4338 0.034 Uiso 1 1 calc R . .
C30 C 0.1385(3) 0.6368(3) 0.4596(3) 0.0377(8) Uani 1 1 d . . .
H30A H 0.1139 0.6263 0.5224 0.057 Uiso 1 1 calc R . .
H30B H 0.0504 0.6067 0.4001 0.057 Uiso 1 1 calc R . .
H30C H 0.1994 0.7240 0.4720 0.057 Uiso 1 1 calc R . .
C31 C 0.5012(3) 0.7697(2) 0.5080(2) 0.0246(7) Uani 1 1 d . . .
H31A H 0.4928 0.7559 0.4333 0.029 Uiso 1 1 calc R . .
H31B H 0.4562 0.8227 0.5254 0.029 Uiso 1 1 calc R . .
C32 C 0.6588(3) 0.8363(3) 0.5747(3) 0.0412(9) Uani 1 1 d . . .
H32A H 0.6682 0.8527 0.6490 0.062 Uiso 1 1 calc R . .
H32B H 0.7054 0.9140 0.5613 0.062 Uiso 1 1 calc R . .
H32C H 0.7047 0.7851 0.5571 0.062 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'
Ni Ni 0.3393 1.1124 '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'
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
N1 Ga1 N2 86.47(9) . . ?
N1 Ga1 Ni1 137.40(7) . . ?
N2 Ga1 Ni1 135.63(6) . . ?
P1 Ni1 P1 180.0 2_666 . ?
P1 Ni1 Ga1 89.41(3) 2_666 . ?
P1 Ni1 Ga1 90.59(3) . . ?
P1 Ni1 Ga1 90.59(3) 2_666 2_666 ?
P1 Ni1 Ga1 89.41(3) . 2_666 ?
Ga1 Ni1 Ga1 180.0 . 2_666 ?
C31 P1 C27 99.79(13) . . ?
C31 P1 C29 103.41(14) . . ?
C27 P1 C29 101.30(14) . . ?
C31 P1 Ni1 112.68(10) . . ?
C27 P1 Ni1 122.14(9) . . ?
C29 P1 Ni1 114.93(10) . . ?
C1 N1 C3 117.2(2) . . ?
C1 N1 Ga1 109.56(16) . . ?
C3 N1 Ga1 131.40(18) . . ?
C2 N2 C15 116.9(2) . . ?
C2 N2 Ga1 109.50(16) . . ?
C15 N2 Ga1 133.53(17) . . ?
C2 C1 N1 117.3(2) . . ?
C1 C2 N2 117.1(3) . . ?
C4 C3 C8 120.3(2) . . ?
C4 C3 N1 119.5(2) . . ?
C8 C3 N1 120.2(2) . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 C9 121.0(2) . . ?
C3 C4 C9 120.2(2) . . ?
C6 C5 C4 120.7(3) . . ?
C7 C6 C5 120.3(3) . . ?
C6 C7 C8 121.6(3) . . ?
C7 C8 C3 118.3(3) . . ?
C7 C8 C12 119.6(2) . . ?
C3 C8 C12 122.1(2) . . ?
C4 C9 C11 113.5(2) . . ?
C4 C9 C10 110.4(2) . . ?
C11 C9 C10 109.6(3) . . ?
C8 C12 C13 111.4(3) . . ?
C8 C12 C14 112.2(3) . . ?
C13 C12 C14 109.3(3) . . ?
C20 C15 C16 120.3(2) . . ?
C20 C15 N2 119.1(2) . . ?
C16 C15 N2 120.6(2) . . ?
C17 C16 C15 118.1(3) . . ?
C17 C16 C21 118.6(2) . . ?
C15 C16 C21 123.3(2) . . ?
C18 C17 C16 122.2(3) . . ?
C17 C18 C19 119.5(3) . . ?
C18 C19 C20 121.3(3) . . ?
C19 C20 C15 118.6(3) . . ?
C19 C20 C24 120.7(2) . . ?
C15 C20 C24 120.6(2) . . ?
C16 C21 C22 111.1(2) . . ?
C16 C21 C23 112.6(2) . . ?
C22 C21 C23 108.7(2) . . ?
C20 C24 C26 114.0(2) . . ?
C20 C24 C25 110.6(2) . . ?
C26 C24 C25 110.1(3) . . ?
C28 C27 P1 116.6(2) . . ?
C30 C29 P1 117.0(2) . . ?
C32 C31 P1 113.48(19) . . ?
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
Ga1 N1 1.909(2) . ?
Ga1 N2 1.912(2) . ?
Ga1 Ni1 2.3614(7) . ?
Ni1 P1 2.1908(8) 2_666 ?
Ni1 P1 2.1908(8) . ?
Ni1 Ga1 2.3614(7) 2_666 ?
P1 C31 1.829(3) . ?
P1 C27 1.835(3) . ?
P1 C29 1.841(3) . ?
N1 C1 1.398(4) . ?
N1 C3 1.427(3) . ?
N2 C2 1.399(3) . ?
N2 C15 1.434(3) . ?
C1 C2 1.337(4) . ?
C3 C4 1.414(4) . ?
C3 C8 1.417(4) . ?
C4 C5 1.394(4) . ?
C4 C9 1.522(4) . ?
C5 C6 1.388(4) . ?
C6 C7 1.370(4) . ?
C7 C8 1.396(4) . ?
C8 C12 1.519(4) . ?
C9 C11 1.526(4) . ?
C9 C10 1.533(4) . ?
C12 C13 1.528(5) . ?
C12 C14 1.528(5) . ?
C15 C20 1.413(4) . ?
C15 C16 1.416(4) . ?
C16 C17 1.398(4) . ?
C16 C21 1.525(4) . ?
C17 C18 1.365(4) . ?
C18 C19 1.388(4) . ?
C19 C20 1.395(4) . ?
C20 C24 1.520(4) . ?
C21 C22 1.528(4) . ?
C21 C23 1.538(4) . ?
C24 C26 1.528(4) . ?
C24 C25 1.528(4) . ?
C27 C28 1.520(4) . ?
C29 C30 1.530(4) . ?
C31 C32 1.516(4) . ?
