#------------------------------------------------------------------------------
#$Date: 2008-02-21 13:43:11 +0000 (Thu, 21 Feb 2008) $
#$Revision: 129 $
#$URL: svn://www.crystallography.net/cod/cif/4/4000118.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_4000118
_journal_name_full 'Chemistry of Materials'
_journal_year    2002
_chemical_name_systematic
;
 Bis(1,3-diphenyl-1,3-propanediono)bis(4-phenylpyridine)nickel(II),
clathrate with benzene 1:4
;
_chemical_name_common
;
Bis(dibenzoylmethanato)bis-
(4-phenylpyridine)nickel(II), clathrate with benzene 1:4
;
_chemical_formula_moiety          [Ni(4-PhPy)2(DBM)2]*4(benzene)
_chemical_formula_sum     'C76 H64 N2 Ni O4'
_chemical_formula_weight          1128.00
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P-1'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a                    11.565(2)
_cell_length_b                    12.354(2)
_cell_length_c                    13.205(2)
_cell_angle_alpha                 110.34(1)
_cell_angle_beta                  94.32(1)
_cell_angle_gamma                 117.73(1)
_cell_volume                      1500.6(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     'all data'
_cell_measurement_theta_min       1.7
_cell_measurement_theta_max       28.7
_exptl_crystal_description        'oblique block'
_exptl_crystal_colour             brown
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.248
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              594
_exptl_absorpt_coefficient_mu     0.377
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.7066
_exptl_absorpt_correction_T_max   0.9422
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71070
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Smart CCD'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             18011
_diffrn_reflns_av_R_equivalents   0.0234
_diffrn_reflns_av_sigmaI/netI     0.0468
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          1.72
_diffrn_reflns_theta_max          28.73
_reflns_number_total              7717
_reflns_number_gt                 5583
_reflns_threshold_expression      >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          7717
_refine_ls_number_parameters      379
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0654
_refine_ls_R_factor_gt            0.0389
_refine_ls_wR_factor_ref          0.0963
_refine_ls_wR_factor_gt           0.0902
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.021
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
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_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ni Ni 0.0000 0.0000 1.0000 0.02777(9) Uani 1 d S . .
O1 O 0.17949(9) 0.02472(9) 1.06250(8) 0.0326(2) Uani 1 d . . .
C1 C 0.20581(13) -0.06793(13) 1.03917(11) 0.0250(3) Uani 1 d . . .
C11 C 0.35083(13) -0.02194(14) 1.09116(11) 0.0264(3) Uani 1 d . . .
C12 C 0.44119(15) 0.11499(15) 1.16104(13) 0.0361(3) Uani 1 d . . .
H12 H 0.4108 0.1768 1.1743 0.043 Uiso 1 calc R . .
C13 C 0.57528(15) 0.16233(17) 1.21156(14) 0.0435(4) Uani 1 d . . .
H13 H 0.6361 0.2562 1.2593 0.052 Uiso 1 calc R . .
C14 C 0.62092(15) 0.07412(17) 1.19306(14) 0.0408(4) Uani 1 d . . .
H14 H 0.7128 0.1067 1.2281 0.049 Uiso 1 calc R . .
C15 C 0.53254(15) -0.06160(17) 1.12345(15) 0.0417(4) Uani 1 d . . .
H15 H 0.5638 -0.1227 1.1099 0.050 Uiso 1 calc R . .
C16 C 0.39838(14) -0.10962(15) 1.07303(13) 0.0345(3) Uani 1 d . . .
H16 H 0.3382 -0.2036 1.0255 0.041 Uiso 1 calc R . .
C2 C 0.11083(13) -0.20703(14) 0.97202(12) 0.0304(3) Uani 1 d . . .
H2 H 0.1445 -0.2663 0.9570 0.036 Uiso 1 calc R . .
O3 O -0.08947(9) -0.20209(9) 0.93143(8) 0.0300(2) Uani 1 d . . .
C3 C -0.02830(13) -0.26566(13) 0.92558(11) 0.0240(3) Uani 1 d . . .
C31 C -0.11893(13) -0.41772(13) 0.86308(11) 0.0249(3) Uani 1 d . . .
C32 C -0.08041(14) -0.50617(14) 0.87112(12) 0.0313(3) Uani 1 d . . .
H32 H 0.0091 -0.4708 0.9141 0.038 Uiso 1 calc R . .
C33 C -0.17080(16) -0.64539(15) 0.81719(14) 0.0377(4) Uani 1 d . . .
H33 H -0.1438 -0.7046 0.8249 0.045 Uiso 1 calc R . .
C34 C -0.30010(16) -0.69824(15) 0.75225(14) 0.0395(4) Uani 1 d . . .
H34 H -0.3618 -0.7937 0.7146 0.047 Uiso 1 calc R . .
C35 C -0.33934(15) -0.61171(15) 0.74228(14) 0.0408(4) Uani 1 d . . .
H35 H -0.4280 -0.6477 0.6972 0.049 Uiso 1 calc R . .
C36 C -0.24979(14) -0.47258(14) 0.79777(13) 0.0324(3) Uani 1 d . . .
H36 H -0.2781 -0.4138 0.7912 0.039 Uiso 1 calc R . .
N7 N 0.05408(11) 0.00121(12) 0.85018(10) 0.0315(3) Uani 1 d . . .
C71 C 0.16502(14) 0.11031(14) 0.85340(13) 0.0330(3) Uani 1 d . . .
H71 H 0.2143 0.1894 0.9230 0.040 Uiso 1 calc R . .
C72 C 0.21051(14) 0.11248(15) 0.76010(13) 0.0342(3) Uani 1 d . . .
H72 H 0.2891 0.1922 0.7663 0.041 Uiso 1 calc R . .
C73 C 0.14171(14) -0.00166(14) 0.65710(12) 0.0315(3) Uani 1 d . . .
C74 C 0.02473(15) -0.11298(15) 0.65374(13) 0.0364(4) Uani 1 d . . .
H74 H -0.0277 -0.1927 0.5849 0.044 Uiso 1 calc R . .
C75 C -0.01482(14) -0.10722(15) 0.75028(13) 0.0358(3) Uani 1 d . . .
H75 H -0.0952 -0.1843 0.7457 0.043 Uiso 1 calc R . .
C76 C 0.19177(15) -0.00409(15) 0.55673(13) 0.0342(3) Uani 1 d . . .
C77 C 0.33147(17) 0.05794(16) 0.56861(14) 0.0416(4) Uani 1 d . . .
H77 H 0.3938 0.0996 0.6408 0.050 Uiso 1 calc R . .
C78 C 0.3799(2) 0.05918(18) 0.47617(16) 0.0509(5) Uani 1 d . . .
H78 H 0.4751 0.1005 0.4849 0.061 Uiso 1 calc R . .
C79 C 0.2908(2) 0.00095(18) 0.37166(17) 0.0547(5) Uani 1 d . . .
H79 H 0.3246 0.0034 0.3086 0.066 Uiso 1 calc R . .
C7X C 0.1522(2) -0.06125(19) 0.35840(15) 0.0520(5) Uani 1 d . . .
H7X H 0.0907 -0.1014 0.2862 0.062 Uiso 1 calc R . .
C7Y C 0.10287(18) -0.06525(17) 0.44994(14) 0.0432(4) Uani 1 d . . .
H7Y H 0.0073 -0.1102 0.4399 0.052 Uiso 1 calc R . .
C1A C 0.8238(2) 0.5855(2) 0.2269(2) 0.0665(6) Uani 1.0000(19) d . A 1
H1A H 0.9188 0.6310 0.2617 0.080 Uiso 1.0000(19) calc R A 1
C2A C 0.7772(3) 0.5455(3) 0.1153(2) 0.0791(8) Uani 1.0000(19) d . A 1
H2A H 0.8398 0.5647 0.0721 0.095 Uiso 1.0000(19) calc R A 1
C3A C 0.6406(3) 0.4777(3) 0.06449(19) 0.0872(9) Uani 1.0000(19) d . A 1
H3A H 0.6083 0.4490 -0.0140 0.105 Uiso 1.0000(19) calc R A 1
C4A C 0.5496(2) 0.4509(2) 0.1272(2) 0.0743(7) Uani 1.0000(19) d . A 1
H4A H 0.4544 0.4033 0.0923 0.089 Uiso 1.0000(19) calc R A 1
C5A C 0.5977(2) 0.4935(2) 0.23986(18) 0.0596(5) Uani 1.0000(19) d . A 1
H5A H 0.5360 0.4767 0.2841 0.072 Uiso 1.0000(19) calc R A 1
C6A C 0.7338(2) 0.5601(2) 0.28898(17) 0.0606(5) Uani 1.0000(19) d . A 1
H6A H 0.7666 0.5892 0.3675 0.073 Uiso 1.0000(19) calc R A 1
C1B C 0.5343(2) 0.40383(19) 0.48155(16) 0.0542(5) Uani 1.006(3) d P . 2
H1B H 0.5580 0.3372 0.4685 0.065 Uiso 1.006(3) calc PR . 2
C2B C 0.63380(19) 0.53945(19) 0.54024(15) 0.0512(5) Uani 1.006(3) d P . 2
H2B H 0.7256 0.5661 0.5680 0.061 Uiso 1.006(3) calc PR . 2
C3B C 0.5995(2) 0.63597(19) 0.55845(16) 0.0547(5) Uani 1.006(3) d P . 2
H3B H 0.6677 0.7296 0.5984 0.066 Uiso 1.006(3) calc PR . 2
C1C C -0.06335(18) 0.45522(19) 0.57393(15) 0.0507(5) Uani 1.010(3) d P . 3
H1C H -0.1072 0.4245 0.6249 0.061 Uiso 1.010(3) calc PR . 3
C2C C 0.0470(2) 0.5850(2) 0.61303(15) 0.0578(6) Uani 1.010(3) d P . 3
H2C H 0.0800 0.6439 0.6913 0.069 Uiso 1.010(3) calc PR . 3
C3C C 0.11014(18) 0.63006(19) 0.53932(15) 0.0537(5) Uani 1.010(3) d P . 3
H3C H 0.1860 0.7201 0.5667 0.064 Uiso 1.010(3) calc PR . 3
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ni 0.02368(14) 0.02104(13) 0.03175(16) 0.00588(11) 0.00115(10) 0.01168(11)
O1 0.0266(5) 0.0232(5) 0.0379(6) 0.0051(4) -0.0002(4) 0.0129(4)
C1 0.0239(6) 0.0258(7) 0.0236(7) 0.0102(6) 0.0057(5) 0.0124(6)
C11 0.0238(6) 0.0301(7) 0.0239(7) 0.0117(6) 0.0055(5) 0.0133(6)
C12 0.0303(7) 0.0313(8) 0.0376(9) 0.0078(7) 0.0026(6) 0.0158(6)
C13 0.0276(8) 0.0356(8) 0.0448(10) 0.0053(7) -0.0021(7) 0.0106(7)
C14 0.0248(7) 0.0490(10) 0.0397(9) 0.0144(8) 0.0008(6) 0.0175(7)
C15 0.0326(8) 0.0438(9) 0.0522(10) 0.0189(8) 0.0061(7) 0.0248(7)
C16 0.0282(7) 0.0301(7) 0.0390(9) 0.0104(7) 0.0023(6) 0.0150(6)
C2 0.0262(7) 0.0241(7) 0.0372(8) 0.0085(6) 0.0037(6) 0.0147(6)
O3 0.0250(5) 0.0227(5) 0.0356(6) 0.0065(4) 0.0017(4) 0.0129(4)
C3 0.0271(7) 0.0228(6) 0.0214(7) 0.0090(5) 0.0064(5) 0.0129(6)
C31 0.0265(7) 0.0232(6) 0.0229(7) 0.0087(5) 0.0074(5) 0.0125(6)
C32 0.0301(7) 0.0273(7) 0.0321(8) 0.0096(6) 0.0036(6) 0.0149(6)
C33 0.0411(8) 0.0253(7) 0.0460(9) 0.0131(7) 0.0094(7) 0.0190(7)
C34 0.0368(8) 0.0206(7) 0.0461(10) 0.0079(7) 0.0062(7) 0.0095(6)
C35 0.0295(8) 0.0287(8) 0.0484(10) 0.0097(7) -0.0014(7) 0.0106(7)
C36 0.0296(7) 0.0260(7) 0.0379(8) 0.0108(6) 0.0043(6) 0.0148(6)
N7 0.0266(6) 0.0268(6) 0.0345(7) 0.0089(5) 0.0015(5) 0.0134(5)
C71 0.0289(7) 0.0262(7) 0.0341(8) 0.0070(6) 0.0025(6) 0.0126(6)
C72 0.0281(7) 0.0285(7) 0.0381(9) 0.0106(7) 0.0047(6) 0.0124(6)
C73 0.0295(7) 0.0316(7) 0.0339(8) 0.0122(6) 0.0034(6) 0.0186(6)
C74 0.0340(8) 0.0304(8) 0.0303(8) 0.0058(6) -0.0011(6) 0.0132(7)
C75 0.0274(7) 0.0285(7) 0.0361(9) 0.0090(7) -0.0002(6) 0.0084(6)
C76 0.0413(8) 0.0277(7) 0.0345(8) 0.0110(6) 0.0086(7) 0.0209(7)
C77 0.0434(9) 0.0353(8) 0.0418(9) 0.0151(7) 0.0132(7) 0.0186(7)
C78 0.0572(11) 0.0372(9) 0.0564(12) 0.0203(9) 0.0275(9) 0.0219(8)
C79 0.0912(15) 0.0437(10) 0.0500(12) 0.0254(9) 0.0389(11) 0.0444(11)
C7X 0.0809(14) 0.0560(11) 0.0349(10) 0.0170(8) 0.0152(9) 0.0496(11)
C7Y 0.0524(10) 0.0464(9) 0.0374(9) 0.0136(8) 0.0088(8) 0.0345(9)
C1A 0.0574(12) 0.0766(15) 0.0784(16) 0.0421(13) 0.0335(12) 0.0367(11)
C2A 0.117(2) 0.127(2) 0.0852(18) 0.0763(17) 0.0741(17) 0.104(2)
C3A 0.148(2) 0.129(2) 0.0433(13) 0.0376(14) 0.0293(15) 0.115(2)
C4A 0.0718(15) 0.0860(17) 0.0649(15) 0.0267(13) 0.0074(12) 0.0472(13)
C5A 0.0514(11) 0.0781(15) 0.0643(14) 0.0428(12) 0.0268(10) 0.0349(11)
C6A 0.0595(12) 0.0716(14) 0.0472(11) 0.0254(10) 0.0206(10) 0.0315(11)
C1B 0.0702(13) 0.0480(11) 0.0545(12) 0.0249(9) 0.0201(10) 0.0363(10)
C2B 0.0519(10) 0.0555(11) 0.0462(11) 0.0260(9) 0.0126(8) 0.0256(9)
C3B 0.0611(12) 0.0401(10) 0.0491(11) 0.0159(8) 0.0094(9) 0.0198(9)
C1C 0.0506(11) 0.0573(11) 0.0418(10) 0.0217(9) 0.0150(8) 0.0262(9)
C2C 0.0595(12) 0.0511(11) 0.0346(10) 0.0055(8) 0.0074(8) 0.0186(9)
C3C 0.0470(10) 0.0430(10) 0.0479(11) 0.0112(8) 0.0076(8) 0.0137(8)