#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:09:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179364 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/61/4326193.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_4326193
loop_
_publ_author_name
'Chao Chen'
'Huayu Qiu'
'Wanzhi Chen'
_publ_section_title
;
 Synthesis and Characterization of Nickel Inverse 9-Metallacrown-3,
 Palladium-Silver, and Dinuclear Platinum Complexes Containing
 Pyrazole-Functionalized NHC Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8671
_journal_page_last               8678
_journal_paper_doi               10.1021/ic2012233
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C36 H36 F12 N18 Ni3 O2 P2 S0'
_chemical_formula_weight         1218.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.9966(14)
_cell_length_b                   12.9966(14)
_cell_length_c                   16.4807(16)
_cell_measurement_temperature    298(2)
_cell_volume                     2410.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  '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  0.1963
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10137
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.7865
_exptl_absorpt_correction_T_min  0.7325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.144
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_gt           0.1076
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2818
_refine_ls_wR_factor_ref         0.3353
_reflns_number_gt                1510
_reflns_number_total             2823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012233_si_002_3.cif
_cod_data_source_block           3
_cod_database_code               4326193
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
Ni1 Ni 0.12326(11) 0.15113(11) 0.21078(8) 0.0426(6) Uani 1 1 d . . .
H1A H 0.0000 0.0000 0.1186 0.00(6) Uiso 0.50 3 d SPR A 2
O1 O 0.0000 0.0000 0.1684(7) 0.050(3) Uani 1 3 d S . .
O2 O 0.954(3) 0.215(3) 0.9887(14) 0.131(9) Uani 0.50 1 d P . .
H2C H 0.8814 0.1619 0.9950 0.00(4) Uiso 0.50 1 d PR . .
H2D H 0.9951 0.1815 0.9895 0.00(4) Uiso 0.50 1 d PR . .
N1 N 0.2269(7) 0.3448(8) 0.3263(6) 0.048(2) Uani 1 1 d . . .
N2 N 0.3556(8) 0.3338(8) 0.2522(6) 0.052(2) Uani 1 1 d . . .
N3 N 0.2269(8) 0.0956(7) 0.2047(6) 0.048(2) Uani 1 1 d . . .
N4 N 0.1906(8) -0.0212(7) 0.1965(6) 0.049(2) Uani 1 1 d . . .
N5 N 0.0483(8) 0.1937(8) 0.3750(6) 0.053(2) Uani 1 1 d . . .
N6 N 0.1005(8) 0.3948(8) 0.3926(6) 0.057(3) Uani 1 1 d . . .
C1 C 0.2387(9) 0.2802(9) 0.2657(7) 0.047(3) Uani 1 1 d . . .
C2 C 0.3356(10) 0.4402(11) 0.3463(8) 0.057(3) Uani 1 1 d . . .
H2 H 0.3502 0.4988 0.3844 0.000(16) Uiso 1 1 calc R . .
C3 C 0.4140(11) 0.4328(11) 0.3016(8) 0.062(3) Uani 1 1 d . . .
H3 H 0.4956 0.4851 0.3027 0.000(15) Uiso 1 1 calc R . .
C4 C 0.4098(10) 0.2908(9) 0.1945(8) 0.051(3) Uani 1 1 d . . .
H4A H 0.4922 0.3206 0.2091 0.000(15) Uiso 1 1 calc R . .
H4B H 0.4077 0.3199 0.1407 0.000(15) Uiso 1 1 calc R . .
C5 C 0.3457(9) 0.1597(10) 0.1941(7) 0.049(3) Uani 1 1 d . . .
C6 C 0.3874(11) 0.0838(10) 0.1760(7) 0.056(3) Uani 1 1 d . . .
H6 H 0.4653 0.1040 0.1644 0.000(16) Uiso 1 1 calc R . .
C7 C 0.2864(9) -0.0322(9) 0.1789(8) 0.052(3) Uani 1 1 d . . .
C8 C 0.2808(11) -0.1455(10) 0.1637(9) 0.068(4) Uani 1 1 d . . .
H8A H 0.2849 -0.1798 0.2144 0.000(16) Uiso 1 1 calc R . .
H8B H 0.3463 -0.1328 0.1300 0.000(16) Uiso 1 1 calc R . .
H8C H 0.2075 -0.1985 0.1369 0.000(16) Uiso 1 1 calc R . .
C9 C 0.1179(9) 0.3094(9) 0.3671(7) 0.046(3) Uani 1 1 d . . .
C10 C -0.0020(10) 0.3573(10) 0.4298(8) 0.059(3) Uani 1 1 d . . .
H10 H -0.0189 0.4139 0.4503 0.000(16) Uiso 1 1 calc R . .
C11 C -0.0825(12) 0.2432(11) 0.4398(8) 0.059(3) Uani 1 1 d . . .
H11 H -0.1550 0.2192 0.4652 0.000(16) Uiso 1 1 calc R . .
C12 C -0.0525(11) 0.1631(12) 0.4105(7) 0.059(3) Uani 1 1 d . . .
H12 H -0.1070 0.0825 0.4163 0.000(15) Uiso 1 1 calc R . .
P1 P 0.6667 0.3333 0.0256(4) 0.0636(15) Uani 1 3 d S . .
P2 P 0.6667 0.3333 0.3999(5) 0.0738(18) Uani 1 3 d S . .
F1 F 0.6667 0.3333 -0.0699(8) 0.081(4) Uani 1 3 d S B .
F2 F 0.6667 0.3333 0.1219(9) 0.098(5) Uani 1 3 d S B .
F3 F 0.641(11) 0.201(5) 0.030(2) 0.077(9) Uani 0.33 1 d P B 1
F4 F 0.713(12) 0.242(10) 0.033(2) 0.072(10) Uani 0.33 1 d P B 2
F5 F 0.772(10) 0.305(14) 0.022(3) 0.093(14) Uani 0.33 1 d P B 3
F6 F 0.806(6) 0.377(14) 0.025(3) 0.097(19) Uani 0.33 1 d P B 4
F7 F 0.7492(10) 0.3065(9) 0.3427(7) 0.115(3) Uani 1 1 d . . .
F8 F 0.7772(10) 0.4130(10) 0.4528(6) 0.115(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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'
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
N3 Ni1 C1 87.8(4) . .
N3 Ni1 N4 169.5(4) . 2
C1 Ni1 N4 96.0(4) . 2
N3 Ni1 O1 88.8(3) . .
C1 Ni1 O1 170.6(4) . .
N4 Ni1 O1 88.9(3) 2 .
Ni1 O1 Ni1 107.8(4) . 2
Ni1 O1 Ni1 107.8(4) . 3
Ni1 O1 Ni1 107.8(4) 2 3
C1 N1 C2 110.5(9) . .
C1 N1 C9 123.3(9) . .
C2 N1 C9 126.0(10) . .
C1 N2 C3 109.8(10) . .
C1 N2 C4 123.5(10) . .
C3 N2 C4 126.7(9) . .
C5 N3 N4 109.2(9) . .
C5 N3 Ni1 127.4(7) . .
N4 N3 Ni1 122.6(7) . .
N3 N4 C7 108.5(8) . .
N3 N4 Ni1 114.9(7) . 3
C7 N4 Ni1 136.6(7) . 3
C12 N5 C9 113.8(11) . .
C9 N6 C10 114.0(10) . .
N2 C1 N1 104.4(9) . .
N2 C1 Ni1 126.3(9) . .
N1 C1 Ni1 129.3(8) . .
C3 C2 N1 106.8(11) . .
C2 C3 N2 108.4(11) . .
N2 C4 C5 110.2(9) . .
N3 C5 C6 109.0(10) . .
N3 C5 C4 121.5(9) . .
C6 C5 C4 129.2(10) . .
C5 C6 C7 105.5(10) . .
N4 C7 C6 107.8(9) . .
N4 C7 C8 124.0(10) . .
C6 C7 C8 128.2(10) . .
N6 C9 N5 128.8(10) . .
N6 C9 N1 116.4(9) . .
N5 C9 N1 114.8(10) . .
N6 C10 C11 123.8(13) . .
C10 C11 C12 116.1(13) . .
N5 C12 C11 123.5(12) . .
F1 P1 F3 92.5(12) . .
F1 P1 F3 92.5(12) . 2_655
F3 P1 F3 119.82(19) . 2_655
F1 P1 F3 92.5(12) . 3_665
F3 P1 F3 119.82(19) . 3_665
F3 P1 F3 119.82(19) 2_655 3_665
F1 P1 F4 94.5(13) . .
F3 P1 F4 29.8(13) . .
F3 P1 F4 90.1(13) 2_655 .
F3 P1 F4 149.0(12) 3_665 .
F1 P1 F4 94.5(13) . 2_655
F3 P1 F4 149.0(12) . 2_655
F3 P1 F4 29.8(13) 2_655 2_655
F3 P1 F4 90.1(13) 3_665 2_655
F4 P1 F4 119.4(4) . 2_655
F1 P1 F4 94.5(13) . 3_665
F3 P1 F4 90.1(13) . 3_665
F3 P1 F4 149.0(12) 2_655 3_665
F3 P1 F4 29.8(13) 3_665 3_665
F4 P1 F4 119.4(4) . 3_665
F4 P1 F4 119.4(4) 2_655 3_665
F1 P1 F5 88(2) . .
F3 P1 F5 59(2) . .
F3 P1 F5 61(2) 2_655 .
F3 P1 F5 179(2) 3_665 .
F4 P1 F5 29.7(17) . .
F4 P1 F5 91.2(15) 2_655 .
F4 P1 F5 148.9(16) 3_665 .
F1 P1 F5 88(2) . 3_665
F3 P1 F5 61(2) . 3_665
F3 P1 F5 179(2) 2_655 3_665
F3 P1 F5 59(2) 3_665 3_665
F4 P1 F5 91.2(15) . 3_665
F4 P1 F5 148.9(16) 2_655 3_665
F4 P1 F5 29.7(17) 3_665 3_665
F5 P1 F5 119.9(2) . 3_665
F1 P1 F5 88(2) . 2_655
F3 P1 F5 179(2) . 2_655
F3 P1 F5 59(2) 2_655 2_655
F3 P1 F5 61(2) 3_665 2_655
F4 P1 F5 148.9(16) . 2_655
F4 P1 F5 29.7(17) 2_655 2_655
F4 P1 F5 91.2(15) 3_665 2_655
F5 P1 F5 119.9(2) . 2_655
F5 P1 F5 119.9(2) 3_665 2_655
F1 P1 F2 180.000(1) . .
F3 P1 F2 87.5(12) . .
F3 P1 F2 87.5(12) 2_655 .
F3 P1 F2 87.5(12) 3_665 .
F4 P1 F2 85.5(13) . .
F4 P1 F2 85.5(13) 2_655 .
F4 P1 F2 85.5(13) 3_665 .
F5 P1 F2 92(2) . .
F5 P1 F2 92(2) 3_665 .
F5 P1 F2 92(2) 2_655 .
F1 P1 F6 89.7(18) . .
F3 P1 F6 88.3(16) . .
F3 P1 F6 31.9(16) 2_655 .
F3 P1 F6 151.7(16) 3_665 .
F4 P1 F6 58.6(16) . .
F4 P1 F6 61.6(16) 2_655 .
F4 P1 F6 175.6(19) 3_665 .
F5 P1 F6 29.6(16) . .
F5 P1 F6 149.4(16) 3_665 .
F5 P1 F6 90.5(16) 2_655 .
F2 P1 F6 90.3(18) . .
F8 P2 F8 91.5(6) 3_665 .
F8 P2 F8 91.5(6) 3_665 2_655
F8 P2 F8 91.5(6) . 2_655
F8 P2 F7 91.2(5) 3_665 .
F8 P2 F7 88.7(6) . .
F8 P2 F7 177.3(6) 2_655 .
F8 P2 F7 88.7(6) 3_665 3_665
F8 P2 F7 177.3(6) . 3_665
F8 P2 F7 91.2(5) 2_655 3_665
F7 P2 F7 88.6(7) . 3_665
F8 P2 F7 177.3(6) 3_665 2_655
F8 P2 F7 91.2(5) . 2_655
F8 P2 F7 88.7(6) 2_655 2_655
F7 P2 F7 88.6(7) . 2_655
F7 P2 F7 88.6(7) 3_665 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 1.821(9) .
Ni1 C1 1.835(11) .
Ni1 N4 1.866(9) 2
Ni1 O1 1.941(5) .
O1 Ni1 1.941(5) 2
O1 Ni1 1.941(5) 3
N1 C1 1.362(14) .
N1 C2 1.375(14) .
N1 C9 1.422(13) .
N2 C1 1.337(13) .
N2 C3 1.385(16) .
N2 C4 1.451(14) .
N3 C5 1.350(13) .
N3 N4 1.353(11) .
N4 C7 1.354(14) .
N4 Ni1 1.866(9) 3
N5 C12 1.302(14) .
N5 C9 1.318(13) .
N6 C9 1.307(13) .
N6 C10 1.319(15) .
C2 C3 1.298(16) .
C4 C5 1.476(15) .
C5 C6 1.375(15) .
C6 C7 1.421(15) .
C7 C8 1.459(16) .
C10 C11 1.330(16) .
C11 C12 1.370(16) .
P1 F1 1.575(14) .
P1 F3 1.58(4) .
P1 F3 1.58(4) 2_655
P1 F3 1.58(4) 3_665
P1 F4 1.58(4) .
P1 F4 1.58(4) 2_655
P1 F4 1.58(4) 3_665
P1 F5 1.59(5) .
P1 F5 1.59(5) 3_665
P1 F5 1.59(5) 2_655
P1 F2 1.588(16) .
P1 F6 1.61(5) .
P2 F8 1.552(13) 3_665
P2 F8 1.552(13) .
P2 F8 1.552(13) 2_655
P2 F7 1.592(12) .
P2 F7 1.592(12) 3_665
P2 F7 1.592(12) 2_655
