#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:37:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179854 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/50/7015009.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_7015009
loop_
_publ_author_name
'Albrecht, Carolin'
'Bode, Maren'
'Pérez, Janaina Marinas'
'Daniels, Jörg'
'Schnakenburg, Gregor'
'Streubel, Rainer'
_publ_section_title
;
 First examples of oxaphosphirane pentacarbonylchromium(0) and
 -molybdenum(0) complexes: synthesis, structures and reactions
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2654
_journal_paper_doi               10.1039/c0dt01509a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C19 H25 Mo O6 P Si2'
_chemical_formula_sum            'C19 H25 Mo O6 P Si2'
_chemical_formula_weight         532.48
_chemical_name_systematic
;
?
;
_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                87.1032(12)
_cell_angle_beta                 88.3077(13)
_cell_angle_gamma                68.9673(17)
_cell_formula_units_Z            2
_cell_length_a                   8.8987(2)
_cell_length_b                   10.6956(3)
_cell_length_c                   13.9288(5)
_cell_measurement_reflns_used    5395
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1235.70(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18795
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.8691
_exptl_absorpt_correction_T_min  0.7611
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yellowish'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0071P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                4379
_reflns_number_total             6450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01509A.TXT
_cod_data_source_block           Greg116
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_database_code               7015009
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7809(3) 0.5146(2) 0.86255(16) 0.0261(6) Uani 1 1 d . . .
H1A H 0.8611 0.4221 0.8747 0.031 Uiso 1 1 calc R . .
C2 C 0.8286(3) 0.6240(2) 0.89625(17) 0.0262(6) Uani 1 1 d . . .
C3 C 0.9839(3) 0.6201(3) 0.8793(2) 0.0448(8) Uani 1 1 d . . .
H3A H 1.0598 0.5465 0.8479 0.054 Uiso 1 1 calc R . .
C4 C 1.0289(4) 0.7229(3) 0.9079(2) 0.0578(9) Uani 1 1 d . . .
H4A H 1.1355 0.7202 0.8951 0.069 Uiso 1 1 calc R . .
C5 C 0.9222(4) 0.8291(3) 0.9546(2) 0.0507(8) Uani 1 1 d . . .
H5A H 0.9541 0.8999 0.9736 0.061 Uiso 1 1 calc R . .
C6 C 0.7691(4) 0.8321(3) 0.9735(2) 0.0489(8) Uani 1 1 d . . .
H6A H 0.6946 0.9047 1.0066 0.059 Uiso 1 1 calc R . .
C7 C 0.7224(3) 0.7295(3) 0.94470(18) 0.0349(6) Uani 1 1 d . . .
H7A H 0.6162 0.7320 0.9585 0.042 Uiso 1 1 calc R . .
C8 C 0.6876(2) 0.3700(2) 0.71746(16) 0.0219(5) Uani 1 1 d . . .
H8A H 0.6217 0.3908 0.6578 0.026 Uiso 1 1 calc R . .
C9 C 0.3738(3) 0.3694(3) 0.81006(19) 0.0431(8) Uani 1 1 d . . .
H9A H 0.3251 0.3962 0.7466 0.065 Uiso 1 1 calc R . .
H9B H 0.3621 0.4497 0.8451 0.065 Uiso 1 1 calc R . .
H9C H 0.3198 0.3162 0.8461 0.065 Uiso 1 1 calc R . .
C10 C 0.6084(4) 0.1143(3) 0.7312(2) 0.0664(10) Uani 1 1 d . . .
H10A H 0.7222 0.0577 0.7247 0.100 Uiso 1 1 calc R . .
H10B H 0.5612 0.1403 0.6672 0.100 Uiso 1 1 calc R . .
H10C H 0.5509 0.0643 0.7677 0.100 Uiso 1 1 calc R . .
C11 C 0.6862(3) 0.2160(3) 0.91499(18) 0.0425(8) Uani 1 1 d . . .
H11A H 0.6609 0.2948 0.9540 0.064 Uiso 1 1 calc R . .
H11B H 0.8031 0.1746 0.9066 0.064 Uiso 1 1 calc R . .
H11C H 0.6449 0.1512 0.9474 0.064 Uiso 1 1 calc R . .
C12 C 0.9870(3) 0.4100(3) 0.62566(19) 0.0472(8) Uani 1 1 d . . .
H12A H 0.9862 0.4677 0.6782 0.071 Uiso 1 1 calc R . .
H12B H 0.9219 0.4645 0.5727 0.071 Uiso 1 1 calc R . .
H12C H 1.0979 0.3651 0.6030 0.071 Uiso 1 1 calc R . .
C13 C 0.8903(3) 0.1810(3) 0.56729(19) 0.0515(8) Uani 1 1 d . . .
H13A H 0.8064 0.2363 0.5231 0.077 Uiso 1 1 calc R . .
H13B H 0.8646 0.1033 0.5914 0.077 Uiso 1 1 calc R . .
H13C H 0.9943 0.1502 0.5333 0.077 Uiso 1 1 calc R . .
C14 C 1.0394(3) 0.1694(3) 0.76187(18) 0.0426(7) Uani 1 1 d . . .
H14A H 1.0025 0.0957 0.7812 0.064 Uiso 1 1 calc R . .
H14B H 1.0397 0.2207 0.8181 0.064 Uiso 1 1 calc R . .
H14C H 1.1486 0.1328 0.7348 0.064 Uiso 1 1 calc R . .
C15 C 0.7197(3) 0.7834(2) 0.65888(18) 0.0306(6) Uani 1 1 d . . .
C16 C 0.4267(3) 0.8439(2) 0.78547(19) 0.0311(6) Uani 1 1 d . . .
C17 C 0.3101(3) 0.6902(2) 0.66874(18) 0.0310(6) Uani 1 1 d . . .
C18 C 0.5786(3) 0.6423(2) 0.54016(19) 0.0289(6) Uani 1 1 d . . .
C19 C 0.3953(3) 0.9119(3) 0.58732(18) 0.0280(6) Uani 1 1 d . . .
Mo Mo 0.51133(2) 0.74017(2) 0.664392(15) 0.02222(7) Uani 1 1 d . . .
O1 O 0.61044(17) 0.52898(15) 0.87981(11) 0.0303(4) Uani 1 1 d . . .
O2 O 0.83550(19) 0.80574(17) 0.65307(14) 0.0481(5) Uani 1 1 d . . .
O3 O 0.3699(2) 0.90601(18) 0.85102(13) 0.0493(5) Uani 1 1 d . . .
O4 O 0.19773(19) 0.66209(18) 0.67076(13) 0.0468(5) Uani 1 1 d . . .
O5 O 0.6116(2) 0.58903(18) 0.46862(13) 0.0437(5) Uani 1 1 d . . .
O6 O 0.32931(19) 1.01075(18) 0.54610(13) 0.0437(5) Uani 1 1 d . . .
P P 0.65224(7) 0.53389(6) 0.76168(5) 0.02300(15) Uani 1 1 d . . .
Si1 Si 0.59087(8) 0.26755(7) 0.79565(6) 0.03364(19) Uani 1 1 d . . .
Si2 Si 0.90121(8) 0.28147(7) 0.66963(5) 0.02947(18) Uani 1 1 d . . .
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'
Mo Mo -1.6832 0.6857 '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'
Si Si 0.0817 0.0704 '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
C2 C1 O1 116.06(19) . . ?
C2 C1 P 123.42(18) . . ?
O1 C1 P 60.72(10) . . ?
C2 C1 H1A 115.1 . . ?
O1 C1 H1A 115.1 . . ?
P C1 H1A 115.1 . . ?
C7 C2 C3 118.9(2) . . ?
C7 C2 C1 121.8(2) . . ?
C3 C2 C1 119.3(2) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 121.0(3) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C5 C6 C7 120.2(3) . . ?
C5 C6 H6A 119.9 . . ?
C7 C6 H6A 119.9 . . ?
C2 C7 C6 120.6(2) . . ?
C2 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
P C8 Si1 113.33(11) . . ?
P C8 Si2 114.18(11) . . ?
Si1 C8 Si2 118.16(11) . . ?
P C8 H8A 102.8 . . ?
Si1 C8 H8A 102.8 . . ?
Si2 C8 H8A 102.8 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 Mo 177.9(2) . . ?
O3 C16 Mo 175.8(2) . . ?
O4 C17 Mo 179.7(2) . . ?
O5 C18 Mo 177.7(2) . . ?
O6 C19 Mo 178.1(2) . . ?
C19 Mo C18 89.58(9) . . ?
C19 Mo C16 87.70(9) . . ?
C18 Mo C16 175.74(10) . . ?
C19 Mo C17 91.27(9) . . ?
C18 Mo C17 88.95(9) . . ?
C16 Mo C17 87.84(10) . . ?
C19 Mo C15 90.27(9) . . ?
C18 Mo C15 89.59(9) . . ?
C16 Mo C15 93.70(10) . . ?
C17 Mo C15 177.87(9) . . ?
C19 Mo P 178.67(7) . . ?
C18 Mo P 91.71(7) . . ?
C16 Mo P 91.03(7) . . ?
C17 Mo P 89.09(7) . . ?
C15 Mo P 89.41(7) . . ?
C1 O1 P 68.90(10) . . ?
O1 P C1 50.37(8) . . ?
O1 P C8 107.93(9) . . ?
C1 P C8 108.23(11) . . ?
O1 P Mo 119.01(6) . . ?
C1 P Mo 127.92(8) . . ?
C8 P Mo 121.54(8) . . ?
C11 Si1 C9 110.31(12) . . ?
C11 Si1 C10 108.78(14) . . ?
C9 Si1 C10 108.25(13) . . ?
C11 Si1 C8 113.07(11) . . ?
C9 Si1 C8 107.98(10) . . ?
C10 Si1 C8 108.32(11) . . ?
C13 Si2 C14 109.14(13) . . ?
C13 Si2 C12 108.82(12) . . ?
C14 Si2 C12 108.15(12) . . ?
C13 Si2 C8 108.24(11) . . ?
C14 Si2 C8 113.26(10) . . ?
C12 Si2 C8 109.15(10) . . ?
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
C1 C2 1.481(3) . ?
C1 O1 1.482(2) . ?
C1 P 1.795(2) . ?
C1 H1A 1.0000 . ?
C2 C7 1.377(3) . ?
C2 C3 1.382(3) . ?
C3 C4 1.377(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.371(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.369(3) . ?
C5 H5A 0.9500 . ?
C6 C7 1.385(3) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 P 1.804(2) . ?
C8 Si1 1.904(2) . ?
C8 Si2 1.911(2) . ?
C8 H8A 1.0000 . ?
C9 Si1 1.856(2) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 Si1 1.865(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si1 1.855(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 Si2 1.867(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 Si2 1.853(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 Si2 1.865(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O2 1.139(2) . ?
C15 Mo 2.064(2) . ?
C16 O3 1.150(3) . ?
C16 Mo 2.039(3) . ?
C17 O4 1.142(3) . ?
C17 Mo 2.043(2) . ?
C18 O5 1.151(3) . ?
C18 Mo 2.030(3) . ?
C19 O6 1.143(3) . ?
C19 Mo 2.024(3) . ?
Mo P 2.4675(7) . ?
O1 P 1.6786(16) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11A O1 0.98 2.55 3.184(3) 122.4 .
C9 H9B O1 0.98 2.70 3.340(3) 123.3 .
