#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2009003.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009003
loop_
_publ_author_name
'Roh, S.-G.'
'Jeong, J. H.'
_publ_section_title
;
 Dichloro[(cyclopentadienyl)tris(dimethylphosphito-<i>P</i>)cobalt(III)-<i>O</i>,<i>O</i>',<i>O</i>'']oxomolybdenum(V)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1658
_journal_page_last               1660
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Co Mo (C5 H5) (C2 H6 O3 P)3 Cl2 O]'
_chemical_formula_sum            'C11 H23 Cl2 Co Mo O10 P3'
_chemical_formula_weight         633.97
_chemical_name_systematic
;
Dichloro[(cyclopentadienyl)tris(dimethylphosphito-P)
cobalt-O,O',O'']oxomolybdenum(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.244(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7378(5)
_cell_length_b                   14.9883(7)
_cell_length_c                   15.4828(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2223.7(2)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'Molen (Fair, 1990)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_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  0.011
_diffrn_reflns_av_sigmaI/netI    0.019
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3999
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   '(Fair, 1990)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0601P)^2^+4.7336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.108
_reflns_number_gt                3466
_reflns_number_total             3858
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    cf1313.cif
_[local]_cod_data_source_block   VRN00135
_[local]_cod_cif_authors_sg_H-M  P21/n
_cod_database_code               2009003
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mo 0.15855(4) 0.19986(2) 0.65298(2) 0.03040(13) Uani d . 1 . . Mo
Co -0.07489(6) 0.18345(4) 0.84687(4) 0.03325(16) Uani d . 1 . . Co
P1 0.07626(13) 0.28526(8) 0.83604(7) 0.0382(3) Uani d . 1 A . P
P2 -0.15535(11) 0.18586(8) 0.70789(7) 0.0373(3) Uani d . 1 B . P
P3 0.07548(12) 0.08371(8) 0.82715(8) 0.0384(3) Uani d . 1 C . P
Cl1 0.40161(12) 0.19196(9) 0.69122(9) 0.0509(3) Uani d . 1 . . Cl
Cl2 0.15080(14) 0.08380(9) 0.55129(8) 0.0534(3) Uani d . 1 . . Cl
O 0.1453(4) 0.2880(2) 0.5795(2) 0.0458(8) Uani d . 1 . . O
O1 0.1523(3) 0.2825(2) 0.75807(19) 0.0371(7) Uani d . 1 . . O
O2 -0.0524(3) 0.1887(2) 0.64465(19) 0.0385(7) Uani d . 1 . . O
O3 0.1555(3) 0.0988(2) 0.75303(19) 0.0376(7) Uani d . 1 . . O
O4 0.1936(5) 0.2885(4) 0.9202(2) 0.0903(18) Uani d . 1 . . O
C4A 0.3462(12) 0.2822(9) 0.9206(8) 0.053(3) Uiso d P 0.50 A 1 C
H4A 0.3691 0.3160 0.8724 0.080 Uiso calc PR 0.50 A 1 H
H4B 0.3714 0.2208 0.9146 0.080 Uiso calc PR 0.50 A 1 H
H4C 0.3964 0.3055 0.9748 0.080 Uiso calc PR 0.50 A 1 H
C4B 0.3294(12) 0.3169(8) 0.9232(8) 0.050(3) Uiso d P 0.50 A 2 C
H4D 0.3874 0.2935 0.9748 0.074 Uiso calc PR 0.50 A 2 H
H4E 0.3324 0.3809 0.9248 0.074 Uiso calc PR 0.50 A 2 H
H4F 0.3626 0.2961 0.8720 0.074 Uiso calc PR 0.50 A 2 H
O5 0.0017(5) 0.3792(3) 0.8329(3) 0.0826(15) Uani d . 1 . . O
C5A 0.0778(14) 0.4576(9) 0.8293(10) 0.066(3) Uiso d P 0.50 A 1 C
H5A 0.1370 0.4513 0.7863 0.099 Uiso calc PR 0.50 A 1 H
H5B 0.1339 0.4690 0.8857 0.099 Uiso calc PR 0.50 A 1 H
H5C 0.0147 0.5065 0.8134 0.099 Uiso calc PR 0.50 A 1 H
C5B 0.0471(13) 0.4579(9) 0.7925(9) 0.059(3) Uiso d P 0.50 A 2 C
H5D 0.0064 0.5098 0.8142 0.088 Uiso calc PR 0.50 A 2 H
H5E 0.0181 0.4543 0.7300 0.088 Uiso calc PR 0.50 A 2 H
H5F 0.1470 0.4621 0.8063 0.088 Uiso calc PR 0.50 A 2 H
O6 -0.2522(4) 0.1013(3) 0.6839(2) 0.0673(12) Uani d . 1 . . O
C6A -0.3134(13) 0.0793(8) 0.5924(7) 0.051(3) Uiso d P 0.50 B 1 C
H6A -0.2403 0.0735 0.5585 0.077 Uiso calc PR 0.50 B 1 H
H6B -0.3760 0.1260 0.5681 0.077 Uiso calc PR 0.50 B 1 H
H6C -0.3637 0.0241 0.5909 0.077 Uiso calc PR 0.50 B 1 H
C6B -0.2671(16) 0.0550(10) 0.6063(10) 0.070(4) Uiso d P 0.50 B 2 C
H6D -0.3527 0.0218 0.5980 0.106 Uiso calc PR 0.50 B 2 H
H6E -0.1901 0.0146 0.6080 0.106 Uiso calc PR 0.50 B 2 H
H6F -0.2689 0.0961 0.5585 0.106 Uiso calc PR 0.50 B 2 H
O7 -0.2625(5) 0.2635(4) 0.6791(3) 0.0834(15) Uani d . 1 . . O
C7A -0.2221(16) 0.3461(10) 0.6421(10) 0.062(4) Uiso d P 0.50 B 1 C
H7A -0.2082 0.3358 0.5830 0.094 Uiso calc PR 0.50 B 1 H
H7B -0.1370 0.3676 0.6768 0.094 Uiso calc PR 0.50 B 1 H
H7C -0.2944 0.3897 0.6418 0.094 Uiso calc PR 0.50 B 1 H
C7B -0.2612(18) 0.3285(11) 0.6230(11) 0.074(4) Uiso d P 0.50 B 2 C
H7D -0.3167 0.3771 0.6380 0.111 Uiso calc PR 0.50 B 2 H
H7E -0.2989 0.3078 0.5650 0.111 Uiso calc PR 0.50 B 2 H
H7F -0.1670 0.3483 0.6249 0.111 Uiso calc PR 0.50 B 2 H
O8 0.1848(4) 0.0718(4) 0.9161(2) 0.0807(15) Uani d . 1 . . O
C8A 0.3038(13) 0.0174(9) 0.9146(8) 0.059(3) Uiso d P 0.50 C 1 C
H8A 0.3578 0.0419 0.8741 0.088 Uiso calc PR 0.50 C 1 H
H8B 0.2743 -0.0419 0.8964 0.088 Uiso calc PR 0.50 C 1 H
H8C 0.3597 0.0153 0.9723 0.088 Uiso calc PR 0.50 C 1 H
C8B 0.3336(13) 0.0522(9) 0.9232(8) 0.058(3) Uiso d P 0.50 C 2 C
H8D 0.3600 0.0069 0.9669 0.088 Uiso calc PR 0.50 C 2 H
H8E 0.3868 0.1053 0.9399 0.088 Uiso calc PR 0.50 C 2 H
H8F 0.3516 0.0314 0.8677 0.088 Uiso calc PR 0.50 C 2 H
O9 0.0059(5) -0.0111(3) 0.8158(3) 0.0815(15) Uani d . 1 . . O
C9A -0.0076(15) -0.0664(9) 0.7343(9) 0.070(3) Uiso d P 0.50 C 1 C
H9A 0.0752 -0.0601 0.7092 0.106 Uiso calc PR 0.50 C 1 H
H9B -0.0870 -0.0466 0.6928 0.106 Uiso calc PR 0.50 C 1 H
H9C -0.0197 -0.1279 0.7485 0.106 Uiso calc PR 0.50 C 1 H
C9B 0.0466(16) -0.0785(10) 0.7695(10) 0.076(4) Uiso d P 0.50 C 2 C
H9D -0.0184 -0.1270 0.7673 0.114 Uiso calc PR 0.50 C 2 H
H9E 0.1377 -0.0983 0.7970 0.114 Uiso calc PR 0.50 C 2 H
H9F 0.0498 -0.0586 0.7110 0.114 Uiso calc PR 0.50 C 2 H
C11 -0.2780(6) 0.1873(6) 0.8699(4) 0.076(2) Uani d . 1 . . C
H11 -0.3576 0.1926 0.8271 0.092 Uiso calc R 1 . . H
C12 -0.2135(8) 0.1082(4) 0.9011(5) 0.073(2) Uani d . 1 . . C
H12 -0.2405 0.0511 0.8817 0.088 Uiso calc R 1 . . H
C13 -0.1027(7) 0.1293(6) 0.9656(4) 0.075(2) Uani d . 1 . . C
H13 -0.0430 0.0885 0.9986 0.090 Uiso calc R 1 . . H
C14 -0.0945(9) 0.2184(6) 0.9735(4) 0.087(3) Uani d . 1 . . C
H14 -0.0278 0.2498 1.0123 0.104 Uiso calc R 1 . . H
C15 -0.2030(10) 0.2560(5) 0.9136(6) 0.087(3) Uani d . 1 . . C
H15 -0.2211 0.3166 0.9049 0.104 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mo 0.0308(2) 0.0382(2) 0.02524(19) 0.00005(14) 0.01333(14) -0.00083(14)
Co 0.0376(3) 0.0378(3) 0.0288(3) -0.0009(2) 0.0181(2) 0.0001(2)
P1 0.0470(6) 0.0421(6) 0.0301(5) -0.0099(5) 0.0189(5) -0.0093(5)
P2 0.0292(5) 0.0518(7) 0.0334(6) 0.0019(5) 0.0124(4) 0.0020(5)
P3 0.0456(6) 0.0377(6) 0.0364(6) 0.0062(5) 0.0196(5) 0.0099(5)
Cl1 0.0336(6) 0.0649(8) 0.0558(7) -0.0011(5) 0.0119(5) -0.0022(6)
Cl2 0.0640(8) 0.0548(7) 0.0454(6) -0.0043(6) 0.0205(6) -0.0163(5)
O 0.0496(19) 0.060(2) 0.0350(16) -0.0050(16) 0.0268(14) -0.0027(15)
O1 0.0455(17) 0.0394(16) 0.0312(15) -0.0074(13) 0.0198(13) -0.0055(12)
O2 0.0300(15) 0.060(2) 0.0274(14) -0.0003(13) 0.0095(12) -0.0002(13)
O3 0.0435(17) 0.0372(16) 0.0367(16) 0.0062(13) 0.0198(13) 0.0074(13)
O4 0.072(3) 0.169(5) 0.0294(19) -0.057(3) 0.0093(18) -0.010(2)
O5 0.107(4) 0.041(2) 0.122(4) -0.007(2) 0.082(3) -0.011(2)
O6 0.066(2) 0.095(3) 0.045(2) -0.036(2) 0.0202(18) -0.014(2)
O7 0.068(3) 0.109(4) 0.084(3) 0.048(3) 0.042(2) 0.044(3)
O8 0.065(3) 0.137(4) 0.043(2) 0.042(3) 0.0156(18) 0.025(2)
O9 0.111(4) 0.041(2) 0.114(4) -0.011(2) 0.079(3) -0.003(2)
C11 0.044(3) 0.140(7) 0.054(4) 0.010(4) 0.034(3) 0.009(4)
C12 0.090(5) 0.065(4) 0.083(4) -0.029(4) 0.066(4) -0.012(3)
C13 0.070(4) 0.113(6) 0.052(3) 0.021(4) 0.038(3) 0.031(4)
C14 0.097(5) 0.127(7) 0.050(4) -0.049(5) 0.053(4) -0.036(4)
C15 0.124(7) 0.062(4) 0.103(6) 0.024(4) 0.097(6) 0.008(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
Cl Cl 0.1484 0.1585 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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_publ_flag
O Mo O2 93.71(14) yes
O Mo O1 92.96(14) yes
O2 Mo O1 85.88(12) yes
O Mo O3 172.54(13) yes
O2 Mo O3 81.16(12) yes
O1 Mo O3 81.32(12) yes
O Mo Cl1 99.12(12) yes
O2 Mo Cl1 166.73(9) yes
O1 Mo Cl1 90.08(9) yes
O3 Mo Cl1 85.74(9) yes
O Mo Cl2 97.77(12) yes
O2 Mo Cl2 89.12(9) yes
O1 Mo Cl2 168.44(9) yes
O3 Mo Cl2 87.62(9) yes
Cl1 Mo Cl2 92.46(5) yes
C12 Co C15 65.5(3) ?
C12 Co C14 64.7(3) ?
C15 Co C14 39.4(3) ?
C12 Co C11 39.3(3) ?
C15 Co C11 38.7(3) ?
C14 Co C11 65.1(3) ?
C12 Co C13 38.8(3) ?
C15 Co C13 65.0(3) ?
C14 Co C13 37.8(3) ?
C11 Co C13 65.1(3) ?
C12 Co P1 159.0(2) ?
C15 Co P1 98.5(2) ?
C14 Co P1 94.2(2) ?
C11 Co P1 133.0(2) ?
C13 Co P1 123.2(3) ?
C12 Co P3 101.0(2) ?
C15 Co P3 157.5(2) ?
C14 Co P3 119.3(3) ?
C11 Co P3 137.6(2) ?
C13 Co P3 93.1(2) ?
P1 Co P3 89.40(5) yes
C12 Co P2 105.6(2) ?
C15 Co P2 110.2(3) ?
C14 Co P2 149.6(3) ?
C11 Co P2 89.0(2) ?
C13 Co P2 144.2(2) ?
P1 Co P2 92.44(5) yes
P3 Co P2 90.33(5) yes
O1 P1 O4 105.9(2) ?
O1 P1 O5 106.6(2) ?
O4 P1 O5 105.1(3) ?
O1 P1 Co 118.57(13) ?
O4 P1 Co 111.35(18) ?
O5 P1 Co 108.52(17) ?
O2 P2 O7 106.1(2) ?
O2 P2 O6 107.70(19) ?
O7 P2 O6 100.8(3) ?
O2 P2 Co 118.61(13) ?
O7 P2 Co 113.6(2) ?
O6 P2 Co 108.44(15) ?
O3 P3 O9 108.7(2) ?
O3 P3 O8 108.5(2) ?
O9 P3 O8 101.8(3) ?
O3 P3 Co 117.29(13) ?
O9 P3 Co 110.70(18) ?
O8 P3 Co 108.80(17) ?
P1 O1 Mo 136.95(18) ?
P2 O2 Mo 137.07(18) ?
P3 O3 Mo 136.00(17) ?
C4B O4 C4A 21.7(6) ?
C4B O4 P1 125.9(6) ?
C4A O4 P1 125.3(5) ?
C5A O5 C5B 24.1(7) ?
C5A O5 P1 120.5(7) ?
C5B O5 P1 124.6(6) ?
C6B O6 C6A 23.6(7) ?
C6B O6 P2 125.2(7) ?
C6A O6 P2 121.8(5) ?
C7B O7 C7A 20.6(9) ?
C7B O7 P2 130.9(8) ?
C7A O7 P2 122.1(7) ?
C8A O8 C8B 24.0(6) ?
C8A O8 P3 118.2(6) ?
C8B O8 P3 126.1(6) ?
C9B O9 C9A 28.4(7) ?
C9B O9 P3 125.4(7) ?
C9A O9 P3 124.5(6) ?
C15 C11 C12 107.6(7) ?
C15 C11 Co 70.4(3) ?
C12 C11 Co 69.5(3) ?
C13 C12 C11 107.8(6) ?
C13 C12 Co 71.4(3) ?
C11 C12 Co 71.2(3) ?
C14 C13 C12 108.8(7) ?
C14 C13 Co 71.0(4) ?
C12 C13 Co 69.7(3) ?
C13 C14 C15 108.4(7) ?
C13 C14 Co 71.1(4) ?
C15 C14 Co 70.1(3) ?
C11 C15 C14 107.3(6) ?
C11 C15 Co 70.9(3) ?
C14 C15 Co 70.5(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mo O 1.734(3) yes
Mo O2 2.042(3) yes
Mo O1 2.054(3) yes
Mo O3 2.171(3) yes
Mo Cl1 2.3384(12) yes
Mo Cl2 2.3384(12) yes
Co C12 2.050(5) ?
Co C15 2.065(5) ?
Co C14 2.070(6) ?
Co C11 2.071(5) ?
Co C13 2.072(5) ?
Co P1 2.1473(13) yes
Co P3 2.1519(13) yes
Co P2 2.1555(13) yes
P1 O1 1.525(3) yes
P1 O4 1.574(4) ?
P1 O5 1.580(4) ?
P2 O2 1.521(3) yes
P2 O7 1.574(4) ?
P2 O6 1.584(4) ?
P3 O3 1.514(3) yes
P3 O9 1.571(4) ?
P3 O8 1.594(4) ?
O4 C4B 1.382(12) ?
O4 C4A 1.488(13) ?
O5 C5A 1.397(14) ?
O5 C5B 1.442(13) ?
O6 C6B 1.373(15) ?
O6 C6A 1.473(12) ?
O7 C7B 1.306(17) ?
O7 C7A 1.448(15) ?
O8 C8A 1.421(13) ?
O8 C8B 1.463(13) ?
O9 C9B 1.339(15) ?
O9 C9A 1.496(14) ?
C11 C15 1.370(11) ?
C11 C12 1.387(10) ?
C12 C13 1.370(10) ?
C13 C14 1.343(11) ?
C14 C15 1.395(11) ?