#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/90/2009003.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, Soo-Gyun'
'Jeong, Jong Hwa'
_publ_section_title
Dichloro[(cyclopentadienyl)tris(dimethylphosphito-P)cobalt(III)-O,O',O'']oxomolybdenum(V)
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1658
_journal_page_last               1660
_journal_paper_doi               10.1107/S0108270199008781
_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       'ω/2θ 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/[σ²(Fo²)+(0.0601P)²+4.7336P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            cf1313.cif
_cod_data_source_block           VRN00135
_cod_original_sg_symbol_H-M      'P 21/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 .15855(4) .19986(2) .65298(2) .03040(13) Uani d . 1 . . Mo
Co -.07489(6) .18345(4) .84687(4) .03325(16) Uani d . 1 . . Co
P1 .07626(13) .28526(8) .83604(7) .0382(3) Uani d . 1 A . P
P2 -.15535(11) .18586(8) .70789(7) .0373(3) Uani d . 1 B . P
P3 .07548(12) .08371(8) .82715(8) .0384(3) Uani d . 1 C . P
Cl1 .40161(12) .19196(9) .69122(9) .0509(3) Uani d . 1 . . Cl
Cl2 .15080(14) .08380(9) .55129(8) .0534(3) Uani d . 1 . . Cl
O .1453(4) .2880(2) .5795(2) .0458(8) Uani d . 1 . . O
O1 .1523(3) .2825(2) .75807(19) .0371(7) Uani d . 1 . . O
O2 -.0524(3) .1887(2) .64465(19) .0385(7) Uani d . 1 . . O
O3 .1555(3) .0988(2) .75303(19) .0376(7) Uani d . 1 . . O
O4 .1936(5) .2885(4) .9202(2) .0903(18) Uani d . 1 . . O
C4A .3462(12) .2822(9) .9206(8) .053(3) Uiso d P .50 A 1 C
H4A .3691 .3160 .8724 .080 Uiso calc PR .50 A 1 H
H4B .3714 .2208 .9146 .080 Uiso calc PR .50 A 1 H
H4C .3964 .3055 .9748 .080 Uiso calc PR .50 A 1 H
C4B .3294(12) .3169(8) .9232(8) .050(3) Uiso d P .50 A 2 C
H4D .3874 .2935 .9748 .074 Uiso calc PR .50 A 2 H
H4E .3324 .3809 .9248 .074 Uiso calc PR .50 A 2 H
H4F .3626 .2961 .8720 .074 Uiso calc PR .50 A 2 H
O5 .0017(5) .3792(3) .8329(3) .0826(15) Uani d . 1 . . O
C5A .0778(14) .4576(9) .8293(10) .066(3) Uiso d P .50 A 1 C
H5A .1370 .4513 .7863 .099 Uiso calc PR .50 A 1 H
H5B .1339 .4690 .8857 .099 Uiso calc PR .50 A 1 H
H5C .0147 .5065 .8134 .099 Uiso calc PR .50 A 1 H
C5B .0471(13) .4579(9) .7925(9) .059(3) Uiso d P .50 A 2 C
H5D .0064 .5098 .8142 .088 Uiso calc PR .50 A 2 H
H5E .0181 .4543 .7300 .088 Uiso calc PR .50 A 2 H
H5F .1470 .4621 .8063 .088 Uiso calc PR .50 A 2 H
O6 -.2522(4) .1013(3) .6839(2) .0673(12) Uani d . 1 . . O
C6A -.3134(13) .0793(8) .5924(7) .051(3) Uiso d P .50 B 1 C
H6A -.2403 .0735 .5585 .077 Uiso calc PR .50 B 1 H
H6B -.3760 .1260 .5681 .077 Uiso calc PR .50 B 1 H
H6C -.3637 .0241 .5909 .077 Uiso calc PR .50 B 1 H
C6B -.2671(16) .0550(10) .6063(10) .070(4) Uiso d P .50 B 2 C
H6D -.3527 .0218 .5980 .106 Uiso calc PR .50 B 2 H
H6E -.1901 .0146 .6080 .106 Uiso calc PR .50 B 2 H
H6F -.2689 .0961 .5585 .106 Uiso calc PR .50 B 2 H
O7 -.2625(5) .2635(4) .6791(3) .0834(15) Uani d . 1 . . O
C7A -.2221(16) .3461(10) .6421(10) .062(4) Uiso d P .50 B 1 C
H7A -.2082 .3358 .5830 .094 Uiso calc PR .50 B 1 H
H7B -.1370 .3676 .6768 .094 Uiso calc PR .50 B 1 H
H7C -.2944 .3897 .6418 .094 Uiso calc PR .50 B 1 H
C7B -.2612(18) .3285(11) .6230(11) .074(4) Uiso d P .50 B 2 C
H7D -.3167 .3771 .6380 .111 Uiso calc PR .50 B 2 H
H7E -.2989 .3078 .5650 .111 Uiso calc PR .50 B 2 H
H7F -.1670 .3483 .6249 .111 Uiso calc PR .50 B 2 H
O8 .1848(4) .0718(4) .9161(2) .0807(15) Uani d . 1 . . O
C8A .3038(13) .0174(9) .9146(8) .059(3) Uiso d P .50 C 1 C
H8A .3578 .0419 .8741 .088 Uiso calc PR .50 C 1 H
H8B .2743 -.0419 .8964 .088 Uiso calc PR .50 C 1 H
H8C .3597 .0153 .9723 .088 Uiso calc PR .50 C 1 H
C8B .3336(13) .0522(9) .9232(8) .058(3) Uiso d P .50 C 2 C
H8D .3600 .0069 .9669 .088 Uiso calc PR .50 C 2 H
H8E .3868 .1053 .9399 .088 Uiso calc PR .50 C 2 H
H8F .3516 .0314 .8677 .088 Uiso calc PR .50 C 2 H
O9 .0059(5) -.0111(3) .8158(3) .0815(15) Uani d . 1 . . O
C9A -.0076(15) -.0664(9) .7343(9) .070(3) Uiso d P .50 C 1 C
H9A .0752 -.0601 .7092 .106 Uiso calc PR .50 C 1 H
H9B -.0870 -.0466 .6928 .106 Uiso calc PR .50 C 1 H
H9C -.0197 -.1279 .7485 .106 Uiso calc PR .50 C 1 H
C9B .0466(16) -.0785(10) .7695(10) .076(4) Uiso d P .50 C 2 C
H9D -.0184 -.1270 .7673 .114 Uiso calc PR .50 C 2 H
H9E .1377 -.0983 .7970 .114 Uiso calc PR .50 C 2 H
H9F .0498 -.0586 .7110 .114 Uiso calc PR .50 C 2 H
C11 -.2780(6) .1873(6) .8699(4) .076(2) Uani d . 1 . . C
H11 -.3576 .1926 .8271 .092 Uiso calc R 1 . . H
C12 -.2135(8) .1082(4) .9011(5) .073(2) Uani d . 1 . . C
H12 -.2405 .0511 .8817 .088 Uiso calc R 1 . . H
C13 -.1027(7) .1293(6) .9656(4) .075(2) Uani d . 1 . . C
H13 -.0430 .0885 .9986 .090 Uiso calc R 1 . . H
C14 -.0945(9) .2184(6) .9735(4) .087(3) Uani d . 1 . . C
H14 -.0278 .2498 1.0123 .104 Uiso calc R 1 . . H
C15 -.2030(10) .2560(5) .9136(6) .087(3) Uani d . 1 . . C
H15 -.2211 .3166 .9049 .104 Uiso calc R 1 . . H
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_site_symmetry_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) ?
