#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:03:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179229 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/49/4314992.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_4314992
loop_
_publ_author_name
'Xiao-Yi Yi'
'Tony C. H. Lam'
'Ian D. Williams'
'Wa-Hung Leung'
_publ_section_title
;
 Hydrolysis of Bis(p-nitrophenyl)phosphate by Tetravalent Metal Complexes
 with Kläui's Oxygen Tripodal Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2232
_journal_page_last               2238
_journal_paper_doi               10.1021/ic902018u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C34 H70 Ce Co2 N2 O24 P6'
_chemical_formula_weight         1334.72
_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                 110.673(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.351(4)
_cell_length_b                   10.8702(18)
_cell_length_c                   26.204(4)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.15
_cell_volume                     5423.6(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.977
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26583
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0430P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                4742
_reflns_number_total             5210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902018u_si_001_3.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        5423.4(16)
_cod_database_code               4314992
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
Ce1 Ce 0.5000 0.193944(15) 0.2500 0.02638(7) Uani 1 2 d S . .
Co2 Co 0.414378(16) 0.33512(3) 0.081699(12) 0.03029(9) Uani 1 1 d . . .
P1 P 0.51062(3) 0.39517(6) 0.14422(2) 0.03135(14) Uani 1 1 d . . .
P2 P 0.36019(3) 0.33954(6) 0.13893(2) 0.03018(14) Uani 1 1 d . . .
P3 P 0.44300(3) 0.14554(6) 0.10348(2) 0.03194(14) Uani 1 1 d . . .
O1 O 0.57171(9) 0.3518(2) 0.12391(7) 0.0451(4) Uani 1 1 d . . .
O2 O 0.52225(10) 0.54107(17) 0.14423(7) 0.0446(4) Uani 1 1 d . . .
O3 O 0.34853(10) 0.48078(17) 0.14933(8) 0.0443(4) Uani 1 1 d . . .
O4 O 0.28114(9) 0.29144(18) 0.11253(8) 0.0434(4) Uani 1 1 d . . .
O5 O 0.37209(10) 0.06741(17) 0.07884(8) 0.0447(4) Uani 1 1 d . . .
O6 O 0.48795(10) 0.09003(19) 0.06987(7) 0.0479(5) Uani 1 1 d . B .
O7 O 0.52600(8) 0.35633(15) 0.20252(6) 0.0320(3) Uani 1 1 d . . .
O8 O 0.39346(8) 0.27319(16) 0.19239(6) 0.0324(3) Uani 1 1 d . . .
O9 O 0.47983(9) 0.11316(15) 0.16262(6) 0.0338(4) Uani 1 1 d . . .
O10 O 0.42590(10) 0.00485(17) 0.23379(8) 0.0437(4) Uani 1 1 d . . .
O11 O 0.38257(10) 0.13569(18) 0.27379(7) 0.0457(4) Uani 1 1 d . . .
O12 O 0.33259(13) -0.0421(2) 0.25189(11) 0.0709(7) Uani 1 1 d . . .
N1 N 0.37893(12) 0.0313(2) 0.25349(9) 0.0408(5) Uani 1 1 d . . .
C1 C 0.36795(19) 0.4850(3) 0.03358(12) 0.0569(8) Uani 1 1 d . . .
H1A H 0.3538 0.5641 0.0463 0.068 Uiso 1 1 calc R . .
C2 C 0.32527(16) 0.3788(3) 0.01545(11) 0.0547(8) Uani 1 1 d . . .
H2A H 0.2757 0.3697 0.0139 0.066 Uiso 1 1 calc R . .
C3 C 0.36314(18) 0.2910(3) 0.00024(11) 0.0520(8) Uani 1 1 d . . .
H3A H 0.3459 0.2075 -0.0145 0.062 Uiso 1 1 calc R . .
C4 C 0.43015(17) 0.3403(3) 0.00766(11) 0.0535(8) Uani 1 1 d . . .
H4A H 0.4687 0.2980 -0.0009 0.064 Uiso 1 1 calc R . .
C5 C 0.43233(18) 0.4597(3) 0.02775(11) 0.0549(8) Uani 1 1 d . . .
H5A H 0.4730 0.5175 0.0365 0.066 Uiso 1 1 calc R . .
C11 C 0.64526(14) 0.3731(3) 0.15739(12) 0.0492(7) Uani 1 1 d . . .
H11A H 0.6637 0.3032 0.1826 0.059 Uiso 1 1 calc R . .
H11B H 0.6498 0.4490 0.1793 0.059 Uiso 1 1 calc R . .
C12 C 0.68479(16) 0.3855(3) 0.11995(14) 0.0538(7) Uani 1 1 d . . .
H12A H 0.7344 0.4011 0.1411 0.081 Uiso 1 1 calc R . .
H12B H 0.6657 0.4543 0.0949 0.081 Uiso 1 1 calc R . .
H12C H 0.6805 0.3094 0.0990 0.081 Uiso 1 1 calc R . .
C13 C 0.4942(2) 0.6254(3) 0.17381(16) 0.0669(9) Uani 1 1 d . . .
H13A H 0.4433 0.6367 0.1537 0.080 Uiso 1 1 calc R . .
H13B H 0.5001 0.5900 0.2100 0.080 Uiso 1 1 calc R . .
C14 C 0.5288(2) 0.7429(3) 0.1811(2) 0.0798(11) Uani 1 1 d . . .
H14A H 0.5080 0.7982 0.2007 0.120 Uiso 1 1 calc R . .
H14B H 0.5229 0.7782 0.1453 0.120 Uiso 1 1 calc R . .
H14C H 0.5789 0.7323 0.2021 0.120 Uiso 1 1 calc R . .
C15 C 0.3211(2) 0.5137(3) 0.19187(15) 0.0624(9) Uani 1 1 d . . .
H15A H 0.2792 0.4632 0.1883 0.075 Uiso 1 1 calc R . .
H15B H 0.3570 0.4979 0.2282 0.075 Uiso 1 1 calc R . .
C16 C 0.3023(3) 0.6434(4) 0.18647(19) 0.0891(13) Uani 1 1 d . . .
H16A H 0.2843 0.6668 0.2152 0.134 Uiso 1 1 calc R . .
H16B H 0.2661 0.6580 0.1507 0.134 Uiso 1 1 calc R . .
H16C H 0.3440 0.6927 0.1899 0.134 Uiso 1 1 calc R . .
C17 C 0.25613(16) 0.1852(3) 0.13298(12) 0.0492(7) Uani 1 1 d D . .
H17A H 0.2967 0.1366 0.1566 0.059 Uiso 1 1 d R . .
H17B H 0.2286 0.1324 0.1020 0.059 Uiso 1 1 d R . .
C18 C 0.2242(3) 0.2133(6) 0.1725(3) 0.0622(14) Uiso 0.60 1 d PD . .
C18A C 0.1904(5) 0.2339(8) 0.1466(4) 0.061(2) Uiso 0.40 1 d PD . .
C19 C 0.37403(18) -0.0627(3) 0.09163(14) 0.0586(8) Uani 1 1 d . . .
H19A H 0.3708 -0.0740 0.1282 0.070 Uiso 1 1 calc R . .
H19B H 0.4190 -0.0987 0.0922 0.070 Uiso 1 1 calc R . .
C20 C 0.3149(2) -0.1254(3) 0.05029(16) 0.0664(9) Uani 1 1 d . . .
H20A H 0.3165 -0.2134 0.0588 0.100 Uiso 1 1 calc R . .
H20B H 0.3184 -0.1141 0.0142 0.100 Uiso 1 1 calc R . .
H20C H 0.2706 -0.0905 0.0503 0.100 Uiso 1 1 calc R . .
C21 C 0.56081(18) 0.0546(4) 0.09474(15) 0.0718(11) Uani 1 1 d D . .
H21A H 0.5854 0.1175 0.1222 0.086 Uiso 1 1 d R A 1
H21B H 0.5631 -0.0240 0.1144 0.086 Uiso 1 1 d R A 1
C22 C 0.5973(3) 0.0571(6) 0.0566(2) 0.0590(13) Uiso 0.60 1 d PD B .
C22A C 0.5890(6) -0.0237(12) 0.0694(5) 0.087(3) Uiso 0.40 1 d PD B 2
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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
O7 Ce1 O7 81.25(8) 2_655 . ?
O7 Ce1 O8 73.01(6) 2_655 2_655 ?
O7 Ce1 O8 74.34(6) . 2_655 ?
O7 Ce1 O8 74.34(6) 2_655 . ?
O7 Ce1 O8 73.01(6) . . ?
O8 Ce1 O8 136.53(8) 2_655 . ?
O7 Ce1 O9 75.92(6) 2_655 2_655 ?
O7 Ce1 O9 144.17(6) . 2_655 ?
O8 Ce1 O9 72.77(6) 2_655 2_655 ?
O8 Ce1 O9 124.96(6) . 2_655 ?
O7 Ce1 O9 144.17(6) 2_655 . ?
O7 Ce1 O9 75.92(6) . . ?
O8 Ce1 O9 124.96(6) 2_655 . ?
O8 Ce1 O9 72.77(6) . . ?
O9 Ce1 O9 136.10(8) 2_655 . ?
O7 Ce1 O10 118.57(6) 2_655 . ?
O7 Ce1 O10 140.54(6) . . ?
O8 Ce1 O10 141.66(6) 2_655 . ?
O8 Ce1 O10 79.97(6) . . ?
O9 Ce1 O10 75.23(6) 2_655 . ?
O9 Ce1 O10 68.84(6) . . ?
O7 Ce1 O10 140.54(6) 2_655 2_655 ?
O7 Ce1 O10 118.57(6) . 2_655 ?
O8 Ce1 O10 79.97(6) 2_655 2_655 ?
O8 Ce1 O10 141.66(6) . 2_655 ?
O9 Ce1 O10 68.84(6) 2_655 2_655 ?
O9 Ce1 O10 75.23(6) . 2_655 ?
O10 Ce1 O10 69.09(9) . 2_655 ?
O7 Ce1 O11 132.57(6) 2_655 2_655 ?
O7 Ce1 O11 70.93(6) . 2_655 ?
O8 Ce1 O11 63.04(6) 2_655 2_655 ?
O8 Ce1 O11 128.61(6) . 2_655 ?
O9 Ce1 O11 105.56(6) 2_655 2_655 ?
O9 Ce1 O11 63.86(6) . 2_655 ?
O10 Ce1 O11 107.05(6) . 2_655 ?
O10 Ce1 O11 47.72(6) 2_655 2_655 ?
O7 Ce1 O11 70.93(6) 2_655 . ?
O7 Ce1 O11 132.57(6) . . ?
O8 Ce1 O11 128.61(6) 2_655 . ?
O8 Ce1 O11 63.04(6) . . ?
O9 Ce1 O11 63.86(6) 2_655 . ?
O9 Ce1 O11 105.56(6) . . ?
O10 Ce1 O11 47.72(6) . . ?
O10 Ce1 O11 107.05(6) 2_655 . ?
O11 Ce1 O11 153.36(8) 2_655 . ?
C1 Co2 C3 66.42(13) . . ?
C1 Co2 C2 40.11(14) . . ?
C3 Co2 C2 38.59(13) . . ?
C1 Co2 C4 66.28(13) . . ?
C3 Co2 C4 39.82(13) . . ?
C2 Co2 C4 65.78(13) . . ?
C1 Co2 C5 39.36(14) . . ?
C3 Co2 C5 66.19(12) . . ?
C2 Co2 C5 66.04(12) . . ?
C4 Co2 C5 39.22(13) . . ?
C1 Co2 P2 99.82(10) . . ?
C3 Co2 P2 121.81(10) . . ?
C2 Co2 P2 93.81(9) . . ?
C4 Co2 P2 159.49(9) . . ?
C5 Co2 P2 135.62(11) . . ?
C1 Co2 P3 158.76(9) . . ?
C3 Co2 P3 92.42(9) . . ?
C2 Co2 P3 120.87(11) . . ?
C4 Co2 P3 99.01(10) . . ?
C5 Co2 P3 134.74(11) . . ?
P2 Co2 P3 89.65(3) . . ?
C1 Co2 P1 108.66(10) . . ?
C3 Co2 P1 147.23(10) . . ?
C2 Co2 P1 148.74(10) . . ?
C4 Co2 P1 107.58(9) . . ?
C5 Co2 P1 89.37(9) . . ?
P2 Co2 P1 90.87(3) . . ?
P3 Co2 P1 90.01(3) . . ?
O7 P1 O1 110.47(10) . . ?
O7 P1 O2 107.40(10) . . ?
O1 P1 O2 99.24(11) . . ?
O7 P1 Co2 119.44(7) . . ?
O1 P1 Co2 105.28(7) . . ?
O2 P1 Co2 113.12(8) . . ?
O8 P2 O3 110.35(10) . . ?
O8 P2 O4 107.40(9) . . ?
O3 P2 O4 101.62(11) . . ?
O8 P2 Co2 117.67(7) . . ?
O3 P2 Co2 106.54(7) . . ?
O4 P2 Co2 112.09(8) . . ?
O9 P3 O6 107.79(10) . . ?
O9 P3 O5 109.97(10) . . ?
O6 P3 O5 100.81(11) . . ?
O9 P3 Co2 118.96(7) . . ?
O6 P3 Co2 111.60(8) . . ?
O5 P3 Co2 106.18(8) . . ?
C11 O1 P1 120.62(18) . . ?
C13 O2 P1 122.85(18) . . ?
C15 O3 P2 119.23(18) . . ?
C17 O4 P2 122.37(17) . . ?
C19 O5 P3 118.47(18) . . ?
C21 O6 P3 123.27(18) . . ?
P1 O7 Ce1 138.57(9) . . ?
P2 O8 Ce1 142.22(10) . . ?
P3 O9 Ce1 140.17(10) . . ?
N1 O10 Ce1 103.95(14) . . ?
N1 O11 Ce1 92.20(14) . . ?
O12 N1 O11 122.5(3) . . ?
O12 N1 O10 121.3(2) . . ?
O11 N1 O10 116.1(2) . . ?
C5 C1 C2 106.8(3) . . ?
C5 C1 Co2 70.63(17) . . ?
C2 C1 Co2 70.02(17) . . ?
C3 C2 C1 108.8(3) . . ?
C3 C2 Co2 70.68(17) . . ?
C1 C2 Co2 69.87(16) . . ?
C2 C3 C4 108.1(3) . . ?
C2 C3 Co2 70.73(17) . . ?
C4 C3 Co2 70.17(16) . . ?
C5 C4 C3 107.8(3) . . ?
C5 C4 Co2 70.57(16) . . ?
C3 C4 Co2 70.01(16) . . ?
C4 C5 C1 108.6(3) . . ?
C4 C5 Co2 70.21(16) . . ?
C1 C5 Co2 70.01(16) . . ?
O1 C11 C12 107.3(2) . . ?
C14 C13 O2 111.6(3) . . ?
C16 C15 O3 108.8(3) . . ?
C18 C17 O4 114.0(3) . . ?
O4 C17 C18A 104.6(4) . . ?
C18A C18 C17 85.5(9) . . ?
C18 C18A C17 64.1(8) . . ?
O5 C19 C20 109.5(3) . . ?
C22A C21 O6 120.0(6) . . ?
C22 C21 O6 112.3(4) . . ?
C22A C22 C21 63.3(8) . . ?
C22 C22A C21 75.6(9) . . ?
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
Ce1 O7 2.3256(16) 2_655 ?
Ce1 O7 2.3256(16) . ?
Ce1 O8 2.3261(16) 2_655 ?
Ce1 O8 2.3261(16) . ?
Ce1 O9 2.3492(16) 2_655 ?
Ce1 O9 2.3492(16) . ?
Ce1 O10 2.4955(18) . ?
Ce1 O10 2.4955(18) 2_655 ?
Ce1 O11 2.748(2) 2_655 ?
Ce1 O11 2.748(2) . ?
Co2 C1 2.073(3) . ?
Co2 C3 2.074(3) . ?
Co2 C2 2.075(3) . ?
Co2 C4 2.076(3) . ?
Co2 C5 2.081(3) . ?
Co2 P2 2.1529(7) . ?
Co2 P3 2.1627(8) . ?
Co2 P1 2.1634(7) . ?
P1 O7 1.5073(17) . ?
P1 O1 1.587(2) . ?
P1 O2 1.6035(19) . ?
P2 O8 1.5070(17) . ?
P2 O3 1.5917(19) . ?
P2 O4 1.5983(19) . ?
P3 O9 1.5056(17) . ?
P3 O6 1.5954(19) . ?
P3 O5 1.6008(19) . ?
O1 C11 1.462(3) . ?
O2 C13 1.441(4) . ?
O3 C15 1.457(4) . ?
O4 C17 1.440(3) . ?
O5 C19 1.451(3) . ?
O6 C21 1.446(4) . ?
O10 N1 1.269(3) . ?
O11 N1 1.245(3) . ?
O12 N1 1.225(3) . ?
C1 C5 1.399(5) . ?
C1 C2 1.422(5) . ?
C2 C3 1.371(5) . ?
C3 C4 1.413(5) . ?
C4 C5 1.395(5) . ?
C11 C12 1.478(4) . ?
C13 C14 1.438(5) . ?
C15 C16 1.454(5) . ?
C17 C18 1.437(7) . ?
C17 C18A 1.593(10) . ?
C18 C18A 0.809(9) . ?
C19 C20 1.472(4) . ?
C21 C22A 1.328(12) . ?
C21 C22 1.440(7) . ?
C22 C22A 0.976(12) . ?
