#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/73/2227369.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_2227369
loop_
_publ_author_name
'Peulecke, Normen'
'Peitz, Stephan'
'Müller, Bernd H.'
'Spannenberg, Anke'
'Rosenthal, Uwe'
_publ_section_title
;
 [Bis(diphenylphosphanyl)dimethylsilane-κ²P,P']tetracarbonylchromium(0)
;
_journal_coeditor_code           CV2781
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1494
_journal_paper_doi               10.1107/S1600536810043679
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cr (C26 H26 P2 Si) (C O)4]'
_chemical_formula_moiety         'C30 H26 Cr O4 P2 Si'
_chemical_formula_sum            'C30 H26 Cr O4 P2 Si'
_chemical_formula_weight         592.54
_chemical_name_systematic
;
[Bis(diphenylphosphanyl)dimethylsilane-
κ²P,P']tetracarbonylchromium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.073(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7832(4)
_cell_length_b                   11.9204(2)
_cell_length_c                   18.1329(5)
_cell_measurement_reflns_used    13232
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      1.99
_cell_volume                     2913.36(13)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47168
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_correction_T_min  0.7733
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6688
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0259
_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)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                5370
_reflns_number_total             6688
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2781.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227369
_cod_database_fobs_code          2227369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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
C C1 0.25499(13) 0.34671(15) 0.23882(9) 0.0452(4) Uani d . 1 . .
H H1A 0.2964 0.3105 0.2079 0.068 Uiso calc R 1 . .
H H1B 0.2941 0.4035 0.2711 0.068 Uiso calc R 1 . .
H H1C 0.1979 0.3826 0.2060 0.068 Uiso calc R 1 . .
C C2 0.13677(12) 0.12988(15) 0.23902(10) 0.0445(4) Uani d . 1 . .
H H2A 0.0795 0.1647 0.2057 0.067 Uiso calc R 1 . .
H H2B 0.1136 0.0746 0.2714 0.067 Uiso calc R 1 . .
H H2C 0.1782 0.0926 0.2086 0.067 Uiso calc R 1 . .
C C3 0.37225(9) 0.03094(13) 0.35878(8) 0.0312(3) Uani d . 1 . .
C C4 0.38402(12) -0.06394(13) 0.40336(10) 0.0411(4) Uani d D 1 . .
H H4 0.3647 -0.0619 0.4507 0.049 Uiso calc R 1 . .
C C5 0.42314(14) -0.16177(14) 0.38092(10) 0.0525(4) Uani d D 1 . .
H H5 0.4309 -0.2259 0.4127 0.063 Uiso calc R 1 . .
C C6 0.45082(13) -0.16610(15) 0.31233(9) 0.0535(5) Uani d D 1 . .
H H6 0.4776 -0.2332 0.2965 0.064 Uiso calc R 1 . .
C C7 0.43945(13) -0.07262(14) 0.26685(10) 0.0553(5) Uani d D 1 . .
H H7 0.4588 -0.0753 0.2196 0.066 Uiso calc R 1 . .
C C8 0.40018(12) 0.02518(15) 0.28928(9) 0.0442(4) Uani d D 1 . .
H H8 0.3922 0.0889 0.2571 0.053 Uiso calc R 1 . .
C C9 0.43399(9) 0.25333(12) 0.40684(7) 0.0277(3) Uani d . 1 . .
C C10 0.52916(10) 0.20972(14) 0.41518(9) 0.0378(3) Uani d . 1 . .
H H10 0.5384 0.1311 0.4113 0.045 Uiso calc R 1 . .
C C11 0.61087(11) 0.28078(16) 0.42918(10) 0.0455(4) Uani d . 1 . .
H H11 0.6758 0.2503 0.4358 0.055 Uiso calc R 1 . .
C C12 0.59842(12) 0.39468(16) 0.43350(9) 0.0438(4) Uani d . 1 . .
H H12 0.6546 0.4428 0.4432 0.053 Uiso calc R 1 . .
C C13 0.50415(12) 0.43899(14) 0.42375(9) 0.0386(3) Uani d . 1 . .
H H13 0.4952 0.5179 0.4251 0.046 Uiso calc R 1 . .
C C14 0.42244(10) 0.36853(13) 0.41193(8) 0.0330(3) Uani d . 1 . .
H H14 0.3579 0.3994 0.4073 0.040 Uiso calc R 1 . .
C C15 0.13366(9) 0.43218(12) 0.41500(8) 0.0302(3) Uani d . 1 . .
C C16 0.14302(13) 0.51650(14) 0.36418(10) 0.0456(4) Uani d . 1 . .
H H16 0.1494 0.4976 0.3145 0.055 Uiso calc R 1 . .
C C17 0.14317(15) 0.62837(15) 0.38556(12) 0.0561(5) Uani d . 1 . .
H H17 0.1496 0.6854 0.3503 0.067 Uiso calc R 1 . .
C C18 0.13416(12) 0.65736(14) 0.45713(12) 0.0493(4) Uani d . 1 . .
H H18 0.1344 0.7341 0.4714 0.059 Uiso calc R 1 . .
C C19 0.12477(12) 0.57488(15) 0.50772(10) 0.0446(4) Uani d . 1 . .
H H19 0.1183 0.5946 0.5572 0.053 Uiso calc R 1 . .
C C20 0.12470(10) 0.46281(13) 0.48722(9) 0.0355(3) Uani d . 1 . .
H H20 0.1185 0.4064 0.5229 0.043 Uiso calc R 1 . .
C C21 -0.00463(9) 0.25993(12) 0.35370(8) 0.0291(3) Uani d . 1 . .
C C22 -0.06017(11) 0.33304(14) 0.30152(9) 0.0394(3) Uani d . 1 . .
H H22 -0.0289 0.3955 0.2837 0.047 Uiso calc R 1 . .
C C23 -0.16100(12) 0.31502(16) 0.27540(10) 0.0466(4) Uani d . 1 . .
H H23 -0.1985 0.3656 0.2401 0.056 Uiso calc R 1 . .
C C24 -0.20685(11) 0.22462(16) 0.30030(10) 0.0466(4) Uani d . 1 . .
H H24 -0.2760 0.2130 0.2825 0.056 Uiso calc R 1 . .
C C25 -0.15301(11) 0.15113(16) 0.35085(11) 0.0479(4) Uani d . 1 . .
H H25 -0.1847 0.0880 0.3675 0.058 Uiso calc R 1 . .
C C26 -0.05175(11) 0.16869(14) 0.37797(9) 0.0392(3) Uani d . 1 . .
H H26 -0.0149 0.1177 0.4133 0.047 Uiso calc R 1 . .
C C27 0.29769(10) 0.06277(12) 0.55229(8) 0.0303(3) Uani d . 1 . .
C C28 0.16332(10) 0.02616(13) 0.43194(9) 0.0353(3) Uani d . 1 . .
C C29 0.12597(10) 0.16240(13) 0.54054(8) 0.0340(3) Uani d . 1 . .
C C30 0.29387(10) 0.27186(13) 0.53968(8) 0.0318(3) Uani d . 1 . .
Cr Cr1 0.221253(14) 0.156127(18) 0.482132(12) 0.02433(6) Uani d . 1 . .
O O1 0.34093(8) 0.00645(10) 0.59947(6) 0.0440(3) Uani d . 1 . .
O O2 0.13246(10) -0.05665(11) 0.40470(8) 0.0575(3) Uani d . 1 . .
O O3 0.06848(9) 0.16388(12) 0.57808(7) 0.0554(3) Uani d . 1 . .
O O4 0.34046(9) 0.33533(10) 0.57916(7) 0.0500(3) Uani d . 1 . .
P P1 0.32570(2) 0.16071(3) 0.392418(19) 0.02575(8) Uani d . 1 . .
P P2 0.12811(2) 0.28288(3) 0.39145(2) 0.02589(8) Uani d . 1 . .
Si Si1 0.21062(3) 0.23959(3) 0.29856(2) 0.02921(9) Uani d . 1 . .
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'
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'
Cr Cr 0.3209 0.6236 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Si1 C1 H1A . . 109.5 ?
Si1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
Si1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
Si1 C2 H2A . . 109.5 ?
Si1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
Si1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
C4 C3 C8 . . 117.93(14) ?
C4 C3 P1 . . 120.31(11) ?
C8 C3 P1 . . 121.72(12) ?
C3 C4 C5 . . 121.64(15) ?
C3 C4 H4 . . 119.2 ?
C5 C4 H4 . . 119.2 ?
C6 C5 C4 . . 119.81(17) ?
C6 C5 H5 . . 120.1 ?
C4 C5 H5 . . 120.1 ?
C7 C6 C5 . . 119.55(16) ?
C7 C6 H6 . . 120.2 ?
C5 C6 H6 . . 120.2 ?
C6 C7 C8 . . 120.63(16) ?
C6 C7 H7 . . 119.7 ?
C8 C7 H7 . . 119.7 ?
C7 C8 C3 . . 120.44(16) ?
C7 C8 H8 . . 119.8 ?
C3 C8 H8 . . 119.8 ?
C14 C9 C10 . . 118.80(13) ?
C14 C9 P1 . . 120.32(10) ?
C10 C9 P1 . . 120.85(11) ?
C11 C10 C9 . . 120.16(15) ?
C11 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C12 C11 C10 . . 120.47(15) ?
C12 C11 H11 . . 119.8 ?
C10 C11 H11 . . 119.8 ?
C11 C12 C13 . . 119.81(14) ?
C11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
C12 C13 C14 . . 120.08(15) ?
C12 C13 H13 . . 120.0 ?
C14 C13 H13 . . 120.0 ?
C13 C14 C9 . . 120.63(14) ?
C13 C14 H14 . . 119.7 ?
C9 C14 H14 . . 119.7 ?
C16 C15 C20 . . 118.32(14) ?
C16 C15 P2 . . 123.72(12) ?
C20 C15 P2 . . 117.92(11) ?
C15 C16 C17 . . 120.34(17) ?
C15 C16 H16 . . 119.8 ?
C17 C16 H16 . . 119.8 ?
C18 C17 C16 . . 120.68(17) ?
C18 C17 H17 . . 119.7 ?
C16 C17 H17 . . 119.7 ?
C19 C18 C17 . . 119.50(16) ?
C19 C18 H18 . . 120.3 ?
C17 C18 H18 . . 120.3 ?
C18 C19 C20 . . 120.47(17) ?
C18 C19 H19 . . 119.8 ?
C20 C19 H19 . . 119.8 ?
C19 C20 C15 . . 120.70(15) ?
C19 C20 H20 . . 119.7 ?
C15 C20 H20 . . 119.7 ?
C26 C21 C22 . . 118.69(13) ?
C26 C21 P2 . . 119.72(11) ?
C22 C21 P2 . . 121.59(11) ?
C23 C22 C21 . . 120.26(15) ?
C23 C22 H22 . . 119.9 ?
C21 C22 H22 . . 119.9 ?
C24 C23 C22 . . 120.42(15) ?
C24 C23 H23 . . 119.8 ?
C22 C23 H23 . . 119.8 ?
C25 C24 C23 . . 120.02(14) ?
C25 C24 H24 . . 120.0 ?
C23 C24 H24 . . 120.0 ?
C24 C25 C26 . . 120.15(16) ?
C24 C25 H25 . . 119.9 ?
C26 C25 H25 . . 119.9 ?
C21 C26 C25 . . 120.45(15) ?
C21 C26 H26 . . 119.8 ?
C25 C26 H26 . . 119.8 ?
O1 C27 Cr1 . . 175.10(12) ?
O2 C28 Cr1 . . 175.62(14) ?
O3 C29 Cr1 . . 177.97(14) ?
O4 C30 Cr1 . . 174.21(13) ?
C27 Cr1 C29 . . 90.06(6) ?
C27 Cr1 C30 . . 84.22(6) ?
C29 Cr1 C30 . . 90.67(6) ?
C27 Cr1 C28 . . 87.73(7) ?
C29 Cr1 C28 . . 91.71(7) ?
C30 Cr1 C28 . . 171.61(6) ?
C27 Cr1 P1 . . 98.33(4) ?
C29 Cr1 P1 . . 171.42(4) ?
C30 Cr1 P1 . . 91.97(4) ?
C28 Cr1 P1 . . 86.83(5) ?
C27 Cr1 P2 . . 177.47(5) ?
C29 Cr1 P2 . . 91.42(4) ?
C30 Cr1 P2 . . 93.70(4) ?
C28 Cr1 P2 . . 94.28(5) ?
P1 Cr1 P2 . . 80.270(13) ?
C3 P1 C9 . . 103.03(6) ?
C3 P1 Si1 . . 109.81(5) ?
C9 P1 Si1 . . 106.13(5) ?
C3 P1 Cr1 . . 120.78(5) ?
C9 P1 Cr1 . . 120.41(4) ?
Si1 P1 Cr1 . . 95.386(16) ?
C15 P2 C21 . . 102.83(6) ?
C15 P2 Si1 . . 112.95(5) ?
C21 P2 Si1 . . 107.65(5) ?
C15 P2 Cr1 . . 117.58(5) ?
C21 P2 Cr1 . . 120.72(5) ?
Si1 P2 Cr1 . . 94.919(16) ?
C2 Si1 C1 . . 110.61(8) ?
C2 Si1 P1 . . 110.83(6) ?
C1 Si1 P1 . . 117.22(6) ?
C2 Si1 P2 . . 106.93(6) ?
C1 Si1 P2 . . 123.42(6) ?
P1 Si1 P2 . . 85.312(17) ?
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
C1 Si1 . 1.8588(16) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 Si1 . 1.8580(16) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 C4 . 1.380(2) ?
C3 C8 . 1.394(2) ?
C3 P1 . 1.8277(15) ?
C4 C5 . 1.3813(14) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.3760(15) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.3756(15) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3818(15) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
C9 C14 . 1.388(2) ?
C9 C10 . 1.3896(19) ?
C9 P1 . 1.8308(13) ?
C10 C11 . 1.389(2) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.373(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.379(2) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.385(2) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 C16 . 1.388(2) ?
C15 C20 . 1.390(2) ?
C15 P2 . 1.8281(15) ?
C16 C17 . 1.389(3) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.373(3) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.369(3) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.387(2) ?
C19 H19 . 0.9500 ?
C20 H20 . 0.9500 ?
C21 C26 . 1.385(2) ?
C21 C22 . 1.392(2) ?
C21 P2 . 1.8350(13) ?
C22 C23 . 1.388(2) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.373(3) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.369(3) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.395(2) ?
C25 H25 . 0.9500 ?
C26 H26 . 0.9500 ?
C27 O1 . 1.1509(17) ?
C27 Cr1 . 1.8455(14) ?
C28 O2 . 1.1452(19) ?
C28 Cr1 . 1.8874(16) ?
C29 O3 . 1.1477(18) ?
C29 Cr1 . 1.8530(14) ?
C30 O4 . 1.1424(18) ?
C30 Cr1 . 1.8860(15) ?
Cr1 P1 . 2.3877(4) ?
Cr1 P2 . 2.3983(4) ?
P1 Si1 . 2.2731(5) ?
P2 Si1 . 2.2798(5) ?
