#------------------------------------------------------------------------------
#$Date: 2016-03-21 00:21:50 +0100 (lun 21 de mar de 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000099.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_4000099
_journal_name_full               'Chemistry of Materials'
_journal_year                    2001
_chemical_formula_moiety         '[Ni(2-MePy)2(DBM)2]*4/3(benzene)'
_chemical_formula_sum            'C50 H44 N2 Ni O4'
_chemical_formula_weight         795.58
_chemical_name_common            Bis(dibenzoylmethanato)bis(2-methylpyridine)ni
_chemical_name_systematic
;
 Bis(1,3-diphenyl-1,3-propanediono)bis(2-methylpyridine)nickel(II), clathrate wi
;
_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
_cell_angle_alpha                98.920(10)
_cell_angle_beta                 99.230(10)
_cell_angle_gamma                100.290(10)
_cell_formula_units_Z            3
_cell_length_a                   11.765(2)
_cell_length_b                   12.861(2)
_cell_length_c                   21.378(3)
_cell_measurement_reflns_used    'all data'
_cell_measurement_temperature    173(2)
_cell_volume                     3084.7(8)
_diffrn_ambient_temperature      173(2)
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36830
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         15850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                9222
_reflns_number_total             15850
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4000099
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1A Ni 0.407777(19) 0.847912(19) 0.712072(10) 0.03519(7) Uani 1 d . . .
O1A O 0.27102(10) 0.89364(10) 0.74610(5) 0.0376(3) Uani 1 d . . .
C1A C 0.18414(14) 0.91992(13) 0.71366(7) 0.0292(4) Uani 1 d . . .
C11A C 0.08465(14) 0.93260(13) 0.74840(7) 0.0308(4) Uani 1 d . . .
C12A C 0.08360(16) 0.89522(14) 0.80622(8) 0.0362(4) Uani 1 d . . .
H12A H 0.1458 0.8633 0.8231 0.043 Uiso 1 calc R . .
C13A C -0.00719(17) 0.90413(16) 0.83929(8) 0.0443(5) Uani 1 d . . .
H13A H -0.0067 0.8783 0.8786 0.053 Uiso 1 calc R . .
C14A C -0.09785(17) 0.94997(17) 0.81578(9) 0.0501(5) Uani 1 d . . .
H14A H -0.1608 0.9546 0.8382 0.060 Uiso 1 calc R . .
C15A C -0.09679(17) 0.98906(18) 0.75959(9) 0.0520(5) Uani 1 d . . .
H15A H -0.1585 1.0222 0.7436 0.062 Uiso 1 calc R . .
C16A C -0.00684(16) 0.98062(16) 0.72614(9) 0.0429(5) Uani 1 d . . .
H16A H -0.0074 1.0080 0.6873 0.051 Uiso 1 calc R . .
C2A C 0.17707(15) 0.93792(14) 0.65035(8) 0.0352(4) Uani 1 d . . .
H2A H 0.1058 0.9536 0.6301 0.042 Uiso 1 calc R . .
O3A O 0.36275(10) 0.90862(10) 0.63301(5) 0.0364(3) Uani 1 d . . .
C3A C 0.26603(14) 0.93472(13) 0.61469(7) 0.0288(4) Uani 1 d . . .
C31A C 0.25238(14) 0.96352(13) 0.54855(7) 0.0302(4) Uani 1 d . . .
C32A C 0.16624(16) 1.01608(14) 0.52459(8) 0.0384(4) Uani 1 d . . .
H32A H 0.1093 1.0320 0.5495 0.046 Uiso 1 calc R . .
C33A C 0.16261(18) 1.04552(16) 0.46473(9) 0.0466(5) Uani 1 d . . .
H33A H 0.1040 1.0823 0.4491 0.056 Uiso 1 calc R . .
C34A C 0.24355(18) 1.02174(16) 0.42772(9) 0.0479(5) Uani 1 d . . .
H34A H 0.2411 1.0420 0.3867 0.057 Uiso 1 calc R . .
C35A C 0.32802(18) 0.96829(16) 0.45072(8) 0.0477(5) Uani 1 d . . .
H35A H 0.3835 0.9511 0.4251 0.057 Uiso 1 calc R . .
C36A C 0.33315(16) 0.93941(15) 0.51043(8) 0.0380(4) Uani 1 d . . .
H36A H 0.3922 0.9028 0.5257 0.046 Uiso 1 calc R . .
O4A O 0.54178(10) 0.80161(10) 0.67379(5) 0.0411(3) Uani 1 d . . .
C4A C 0.61772(14) 0.75592(13) 0.70070(8) 0.0320(4) Uani 1 d . . .
C41A C 0.70537(15) 0.72486(13) 0.66110(8) 0.0353(4) Uani 1 d . . .
C42A C 0.67575(17) 0.70961(15) 0.59439(9) 0.0433(5) Uani 1 d . . .
H42A H 0.6011 0.7196 0.5747 0.052 Uiso 1 calc R . .
C43A C 0.7531(2) 0.68002(17) 0.55605(10) 0.0545(5) Uani 1 d . . .
H43A H 0.7311 0.6682 0.5104 0.065 Uiso 1 calc R . .
C44A C 0.8625(2) 0.66775(18) 0.58452(11) 0.0619(6) Uani 1 d . . .
H44A H 0.9163 0.6480 0.5584 0.074 Uiso 1 calc R . .
C45A C 0.89379(19) 0.68391(19) 0.65037(11) 0.0646(6) Uani 1 d . . .
H45A H 0.9694 0.6758 0.6698 0.078 Uiso 1 calc R . .
C46A C 0.81561(17) 0.71198(17) 0.68862(10) 0.0501(5) Uani 1 d . . .
H46A H 0.8378 0.7225 0.7342 0.060 Uiso 1 calc R . .
C5A C 0.62338(15) 0.73096(14) 0.76241(8) 0.0360(4) Uani 1 d . . .
H5A H 0.6870 0.6996 0.7780 0.043 Uiso 1 calc R . .
O6A O 0.45399(10) 0.78660(10) 0.79004(5) 0.0410(3) Uani 1 d . . .
C6A C 0.54420(15) 0.74784(13) 0.80330(8) 0.0315(4) Uani 1 d . . .
C61A C 0.56274(15) 0.71604(13) 0.86809(7) 0.0322(4) Uani 1 d . . .
C62A C 0.67319(16) 0.71364(14) 0.90157(8) 0.0369(4) Uani 1 d . . .
H62A H 0.7403 0.7305 0.8827 0.044 Uiso 1 calc R . .
C63A C 0.68657(17) 0.68694(15) 0.96216(8) 0.0433(5) Uani 1 d . . .
H63A H 0.7629 0.6866 0.9847 0.052 Uiso 1 calc R . .
C64A C 0.59108(19) 0.66100(17) 0.98986(9) 0.0505(5) Uani 1 d . . .
H64A H 0.6008 0.6424 1.0314 0.061 Uiso 1 calc R . .
C65A C 0.48055(19) 0.6621(2) 0.95709(10) 0.0616(6) Uani 1 d . . .
H65A H 0.4137 0.6430 0.9758 0.074 Uiso 1 calc R . .
C66A C 0.46662(17) 0.69085(17) 0.89695(9) 0.0506(5) Uani 1 d . . .
H66A H 0.3903 0.6933 0.8753 0.061 Uiso 1 calc R . .
N7A N 0.52702(13) 1.00272(12) 0.75463(7) 0.0402(4) Uani 1 d . . .
C71A C 0.58346(16) 1.04530(16) 0.71070(9) 0.0444(5) Uani 1 d . . .
H71A H 0.5617 1.0094 0.6669 0.053 Uiso 1 calc R . .
C72A C 0.66929(18) 1.13639(17) 0.72602(10) 0.0500(5) Uani 1 d . . .
H72A H 0.7048 1.1641 0.6935 0.060 Uiso 1 calc R . .
C73A C 0.7038(2) 1.18776(17) 0.78969(10) 0.0556(5) Uani 1 d . . .
H73A H 0.7649 1.2505 0.8021 0.067 Uiso 1 calc R . .
C74A C 0.64807(19) 1.14625(17) 0.83452(10) 0.0538(5) Uani 1 d . . .
H74A H 0.6707 1.1803 0.8786 0.065 Uiso 1 calc R . .
C75A C 0.55900(17) 1.05497(16) 0.81617(9) 0.0448(5) Uani 1 d . . .
C76A C 0.49484(19) 1.01213(18) 0.86502(9) 0.0563(6) Uani 1 d . . .
H76A H 0.4127 0.9800 0.8446 0.084 Uiso 1 calc R . .
H76B H 0.4974 1.0711 0.9006 0.084 Uiso 1 calc R . .
H76C H 0.5325 0.9573 0.8817 0.084 Uiso 1 calc R . .
N8A N 0.29554(13) 0.69315(12) 0.65967(7) 0.0415(4) Uani 1 d . . .
C81A C 0.30595(19) 0.67032(17) 0.59674(9) 0.0530(5) Uani 1 d . . .
H81A H 0.3630 0.7182 0.5823 0.064 Uiso 1 calc R . .
C82A C 0.2401(2) 0.58358(19) 0.55322(11) 0.0694(7) Uani 1 d . . .
H82A H 0.2506 0.5710 0.5097 0.083 Uiso 1 calc R . .
C83A C 0.1582(2) 0.5152(2) 0.57449(12) 0.0764(7) Uani 1 d . . .
H83A H 0.1099 0.4544 0.5451 0.092 Uiso 1 calc R . .
C84A C 0.1446(2) 0.53249(18) 0.63678(11) 0.0613(6) Uani 1 d . . .
H84A H 0.0879 0.4843 0.6513 0.074 Uiso 1 calc R . .
C85A C 0.21601(18) 0.62307(17) 0.67947(10) 0.0500(5) Uani 1 d . . .
C86A C 0.2044(2) 0.64231(19) 0.74728(10) 0.0629(6) Uani 1 d . . .
H86A H 0.2723 0.6964 0.7726 0.094 Uiso 1 calc R . .
H86B H 0.2011 0.5750 0.7637 0.094 Uiso 1 calc R . .
H86C H 0.1319 0.6684 0.7509 0.094 Uiso 1 calc R . .
Ni1B Ni 0.0000 0.5000 1.0000 0.03370(8) Uani 1 d S . .
O1B O 0.07817(10) 0.64719(9) 0.99225(6) 0.0379(3) Uani 1 d . . .
C1B C 0.06855(14) 0.73568(13) 1.02428(7) 0.0289(4) Uani 1 d . . .
C11B C 0.14193(15) 0.83368(13) 1.00932(7) 0.0297(4) Uani 1 d . . .
C12B C 0.23384(16) 0.82150(14) 0.97788(8) 0.0393(4) Uani 1 d . . .
H12B H 0.2486 0.7516 0.9657 0.047 Uiso 1 calc R . .
C13B C 0.30494(18) 0.90956(16) 0.96386(10) 0.0507(5) Uani 1 d . . .
H13B H 0.3694 0.9002 0.9435 0.061 Uiso 1 calc R . .
C14B C 0.28200(19) 1.01090(16) 0.97955(9) 0.0507(5) Uani 1 d . . .
H14B H 0.3306 1.0714 0.9700 0.061 Uiso 1 calc R . .
C15B C 0.18889(19) 1.02391(15) 1.00897(9) 0.0502(5) Uani 1 d . . .
H15B H 0.1718 1.0934 1.0188 0.060 Uiso 1 calc R . .
C16B C 0.11937(16) 0.93615(14) 1.02445(8) 0.0395(4) Uani 1 d . . .
H16B H 0.0559 0.9462 1.0456 0.047 Uiso 1 calc R . .
C2B C -0.00392(14) 0.74677(13) 1.06951(8) 0.0313(4) Uani 1 d . . .
H2B H 0.0029 0.8168 1.0937 0.038 Uiso 1 calc R . .
O3B O -0.09879(10) 0.56471(9) 1.05754(5) 0.0353(3) Uani 1 d . . .
C3B C -0.08580(14) 0.66322(13) 1.08212(7) 0.0283(4) Uani 1 d . . .
C31B C -0.17196(14) 0.68784(13) 1.12459(7) 0.0282(4) Uani 1 d . . .
C32B C -0.18909(15) 0.79152(14) 1.14429(8) 0.0355(4) Uani 1 d . . .
H32B H -0.1415 0.8511 1.1332 0.043 Uiso 1 calc R . .
C33B C -0.27492(16) 0.80828(15) 1.17986(9) 0.0431(5) Uani 1 d . . .
H33B H -0.2863 0.8792 1.1927 0.052 Uiso 1 calc R . .
C34B C -0.34373(17) 0.72297(16) 1.19675(9) 0.0462(5) Uani 1 d . . .
H34B H -0.4025 0.7347 1.2212 0.055 Uiso 1 calc R . .
C35B C -0.32693(17) 0.62002(16) 1.17801(9) 0.0459(5) Uani 1 d . . .
H35B H -0.3738 0.5610 1.1900 0.055 Uiso 1 calc R . .
C36B C -0.24242(15) 0.60246(14) 1.14202(8) 0.0357(4) Uani 1 d . . .
H36B H -0.2323 0.5312 1.1290 0.043 Uiso 1 calc R . .
N7B N -0.1419(3) 0.4889(2) 0.91779(15) 0.0382(7) Uani 0.824(4) d P A -1
C71B C -0.2485(2) 0.4457(2) 0.92786(13) 0.0428(6) Uani 0.824(4) d P A -1
H71B H -0.2530 0.4286 0.9692 0.051 Uiso 0.824(4) calc PR A -1
C72B C -0.3513(2) 0.42432(19) 0.88317(12) 0.0502(8) Uani 0.824(4) d P A -1
H72B H -0.4243 0.3931 0.8930 0.060 Uiso 0.824(4) calc PR A -1
C73B C -0.3448(3) 0.4499(3) 0.82326(16) 0.0510(8) Uani 0.824(4) d P A -1
H73B H -0.4136 0.4354 0.7906 0.061 Uiso 0.824(4) calc PR A -1
C74B C -0.2382(3) 0.4964(2) 0.81143(17) 0.0493(7) Uani 0.824(4) d P A -1
H74B H -0.2331 0.5155 0.7706 0.059 Uiso 0.824(4) calc PR A -1
C75B C -0.1370(3) 0.51591(19) 0.85934(13) 0.0424(7) Uani 0.824(4) d P A -1
C76B C -0.0213(3) 0.5681(2) 0.84689(14) 0.0558(8) Uani 0.824(4) d P A -1
H76D H 0.0133 0.6321 0.8804 0.084 Uiso 0.824(4) calc PR A -1
H76E H -0.0328 0.5892 0.8046 0.084 Uiso 0.824(4) calc PR A -1
H76F H 0.0317 0.5173 0.8475 0.084 Uiso 0.824(4) calc PR A -1
N7C N -0.1230(13) 0.5006(12) 0.9044(7) 0.027(3) Uiso 0.176(4) d P A -2
C71C C -0.0640(13) 0.5396(10) 0.8627(5) 0.028(3) Uiso 0.176(4) d P A -2
H71C H 0.0186 0.5666 0.8748 0.033 Uiso 0.176(4) calc PR A -2
C72C C -0.1235(10) 0.5413(9) 0.7996(5) 0.046(3) Uiso 0.176(4) d P A -2
H72C H -0.0810 0.5721 0.7704 0.055 Uiso 0.176(4) calc PR A -2
C73C C -0.2360(12) 0.5010(11) 0.7816(7) 0.040(3) Uiso 0.176(4) d P A -2
H73C H -0.2756 0.4995 0.7390 0.048 Uiso 0.176(4) calc PR A -2
C74C C -0.2933(16) 0.4626(15) 0.8237(9) 0.040(4) Uiso 0.176(4) d P A -2
H74C H -0.3757 0.4350 0.8106 0.049 Uiso 0.176(4) calc PR A -2
C75C C -0.2411(10) 0.4600(8) 0.8861(5) 0.034(3) Uiso 0.176(4) d P A -2
C76C C -0.3030(11) 0.4174(9) 0.9351(5) 0.037(3) Uiso 0.176(4) d P A -2
H76G H -0.2785 0.3511 0.9434 0.055 Uiso 0.176(4) calc PR A -2
H76H H -0.3883 0.4021 0.9190 0.055 Uiso 0.176(4) calc PR A -2
H76I H -0.2832 0.4710 0.9753 0.055 Uiso 0.176(4) calc PR A -2
C1D C -0.5519(2) 0.5810(2) 1.40281(15) 0.0899(9) Uani 1 d . . .
H1D H -0.6109 0.5286 1.4125 0.108 Uiso 1 calc R . .
C2D C -0.5401(2) 0.6861(2) 1.42861(13) 0.0823(8) Uani 1 d . . .
H2D H -0.5897 0.7070 1.4571 0.099 Uiso 1 calc R . .
C3D C -0.4583(2) 0.7615(2) 1.41407(13) 0.0727(7) Uani 1 d . . .
H3D H -0.4509 0.8353 1.4319 0.087 Uiso 1 calc R . .
C4D C -0.3866(2) 0.7316(2) 1.37396(13) 0.0774(7) Uani 1 d . . .
H4D H -0.3295 0.7849 1.3635 0.093 Uiso 1 calc R . .
C5D C -0.3960(2) 0.6256(2) 1.34852(11) 0.0741(7) Uani 1 d . . .
H5D H -0.3445 0.6052 1.3211 0.089 Uiso 1 calc R . .
C6D C -0.4790(3) 0.5494(2) 1.36256(13) 0.0772(8) Uani 1 d . . .
H6D H -0.4866 0.4755 1.3448 0.093 Uiso 1 calc R . .
C1E C -0.0430(14) 0.7593(14) 1.3673(14) 0.101(8) Uani 0.552(15) d P B -1
H1E H -0.1070 0.7901 1.3774 0.121 Uiso 0.552(15) calc PR B -1
C2E C 0.0369(15) 0.7477(12) 1.4178(6) 0.078(6) Uani 0.552(15) d P B -1
H2E H 0.0309 0.7695 1.4615 0.093 Uiso 0.552(15) calc PR B -1
C3E C 0.1262(19) 0.7023(15) 1.4006(10) 0.086(8) Uani 0.552(15) d P B -1
H3E H 0.1888 0.6962 1.4331 0.103 Uiso 0.552(15) calc PR B -1
C4E C 0.1267(15) 0.6655(16) 1.3374(11) 0.084(5) Uani 0.552(15) d P B -1
H4E H 0.1843 0.6262 1.3265 0.101 Uiso 0.552(15) calc PR B -1
C5E C 0.0437(16) 0.6846(14) 1.2883(8) 0.076(4) Uani 0.552(15) d P B -1
H5E H 0.0468 0.6647 1.2440 0.091 Uiso 0.552(15) calc PR B -1
C6E C -0.0406(19) 0.7329(16) 1.3072(9) 0.076(6) Uani 0.552(15) d P B -1
H6E H -0.0992 0.7476 1.2757 0.091 Uiso 0.552(15) calc PR B -1
C1F C -0.0140(16) 0.7584(12) 1.4093(10) 0.064(4) Uani 0.448(15) d P B -2
H1F H -0.0500 0.7820 1.4441 0.076 Uiso 0.448(15) calc PR B -2
C2F C 0.0797(18) 0.7134(15) 1.4233(12) 0.072(5) Uani 0.448(15) d P B -2
H2F H 0.1109 0.7132 1.4671 0.087 Uiso 0.448(15) calc PR B -2
C3F C 0.130(2) 0.6692(17) 1.3770(14) 0.080(6) Uani 0.448(15) d P B -2
H3F H 0.1934 0.6348 1.3876 0.096 Uiso 0.448(15) calc PR B -2
C4F C 0.0878(16) 0.6739(12) 1.3132(10) 0.071(6) Uani 0.448(15) d P B -2
H4F H 0.1253 0.6458 1.2802 0.085 Uiso 0.448(15) calc PR B -2
C5F C -0.008(2) 0.719(2) 1.2976(12) 0.080(8) Uani 0.448(15) d P B -2
H5F H -0.0416 0.7173 1.2537 0.096 Uiso 0.448(15) calc PR B -2
C6F C -0.0602(16) 0.7727(16) 1.3518(11) 0.059(3) Uani 0.448(15) d P B -2
H6F H -0.1202 0.8126 1.3448 0.071 Uiso 0.448(15) calc PR B -2
