#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202431.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_2202431
loop_
_publ_author_name
'Edgar Ocando-Mavarez'
'Julián Ascanio'
'Teresa González'
'Reinaldo Atencio'
'Merlín Rosales'
_publ_section_title
;
 (Acetylacetonato)carbonyl[diallyl(tert-butyl)phosphine]rhodium(I)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m633
_journal_page_last               m635
_journal_paper_doi               10.1107/S1600536803015691
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Rh (C5 H7 O2) (C10 H19 P) (C1 O1)]'
_chemical_formula_moiety         'C16 H26 O3 P Rh'
_chemical_formula_sum            'C16 H26 O3 P Rh'
_chemical_formula_weight         400.25
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.970(2)
_cell_length_b                   12.270(3)
_cell_length_c                   12.758(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.68
_cell_measurement_theta_min      26.42
_cell_volume                     1873.8(7)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular
Structure Corporation, 1991)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation, 1999)
;
_computing_molecular_graphics    SHELXTL-NT
_computing_publication_material  SHELXTL-NT
_computing_structure_refinement  SHELXTL-NT
_computing_structure_solution    'SHELXTL-NT (Bruker, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku AFC-7S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0126
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3098
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.209
_refine_ls_abs_structure_details 'Flack (1983), 956 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0216
_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)+(0.0248P)²+0.2043P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                2580
_reflns_number_total             2795
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf6271.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1873.7(7)
_cod_database_code               2202431
_cod_database_fobs_code          2202431
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
Rh1 0.91546(2) 0.964193(18) 0.12852(2) 0.04217(8) Uani d . 1 . . Rh
P1 1.05392(6) 0.84271(6) 0.14477(7) 0.04182(19) Uani d . 1 . . P
O1 0.8260(2) 0.87419(19) 0.2330(2) 0.0571(6) Uani d . 1 . . O
O2 0.78003(18) 1.07020(15) 0.1194(2) 0.0537(6) Uani d . 1 . . O
O3 1.0552(3) 1.0884(3) -0.0182(3) 0.0970(11) Uani d . 1 . . O
C1 0.7300(3) 0.8948(3) 0.2710(3) 0.0526(8) Uani d . 1 . . C
C2 0.6643(3) 0.9823(3) 0.2434(3) 0.0577(9) Uani d . 1 . . C
H2A 0.5955 0.9880 0.2767 0.069 Uiso calc R 1 . . H
C3 0.6899(3) 1.0634(3) 0.1706(3) 0.0515(9) Uani d . 1 . . C
C4 0.6065(3) 1.1523(3) 0.1506(4) 0.0850(15) Uani d . 1 . . C
H4A 0.6360 1.2021 0.0996 0.127 Uiso calc R 1 . . H
H4B 0.5917 1.1906 0.2147 0.127 Uiso calc R 1 . . H
H4C 0.5384 1.1210 0.1246 0.127 Uiso calc R 1 . . H
C5 0.6914(4) 0.8173(3) 0.3532(4) 0.0806(13) Uani d . 1 . . C
H5A 0.7468 0.7617 0.3632 0.121 Uiso calc R 1 . . H
H5B 0.6224 0.7843 0.3316 0.121 Uiso calc R 1 . . H
H5C 0.6801 0.8558 0.4178 0.121 Uiso calc R 1 . . H
C6 1.0000(3) 1.0407(3) 0.0384(3) 0.0594(9) Uani d . 1 . . C
C7 1.1974(3) 0.8907(3) 0.1247(4) 0.0574(8) Uani d . 1 . . C
H7A 1.2482 0.8316 0.1415 0.069 Uiso calc R 1 . . H
H7B 1.2071 0.9076 0.0509 0.069 Uiso calc R 1 . . H
C8 1.2304(4) 0.9883(3) 0.1872(4) 0.0720(11) Uani d . 1 . . C
H8A 1.1843 1.0492 0.1834 0.086 Uiso calc R 1 . . H
C9 1.3161(5) 0.9950(5) 0.2452(5) 0.113(2) Uani d . 1 . . C
H9A 1.3643 0.9360 0.2512 0.136 Uiso calc R 1 . . H
H9B 1.3307 1.0591 0.2817 0.136 Uiso calc R 1 . . H
C10 1.0552(3) 0.7796(3) 0.2744(3) 0.0580(10) Uani d . 1 . . C
H10A 0.9891 0.7345 0.2813 0.070 Uiso calc R 1 . . H
H10B 1.1197 0.7321 0.2791 0.070 Uiso calc R 1 . . H
C11 1.0584(3) 0.8571(3) 0.3640(3) 0.0640(10) Uani d . 1 . . C
H11A 1.0016 0.9086 0.3676 0.077 Uiso calc R 1 . . H
C12 1.1315(4) 0.8593(4) 0.4361(4) 0.0859(14) Uani d . 1 . . C
H12A 1.1899 0.8093 0.4357 0.103 Uiso calc R 1 . . H
H12B 1.1267 0.9110 0.4893 0.103 Uiso calc R 1 . . H
C13 1.0429(3) 0.7248(3) 0.0526(3) 0.0538(9) Uani d . 1 . . C
C14 1.0500(5) 0.7693(4) -0.0597(3) 0.0863(16) Uani d . 1 . . C
H14A 1.0442 0.7101 -0.1086 0.129 Uiso calc R 1 . . H
H14B 1.1201 0.8059 -0.0693 0.129 Uiso calc R 1 . . H
H14C 0.9899 0.8198 -0.0714 0.129 Uiso calc R 1 . . H
C15 1.1343(4) 0.6397(3) 0.0703(4) 0.0775(13) Uani d . 1 . . C
H15A 1.1249 0.5809 0.0215 0.116 Uiso calc R 1 . . H
H15B 1.1291 0.6120 0.1406 0.116 Uiso calc R 1 . . H
H15C 1.2062 0.6727 0.0602 0.116 Uiso calc R 1 . . H
C16 0.9286(4) 0.6723(3) 0.0698(4) 0.0812(13) Uani d . 1 . . C
H16A 0.9203 0.6112 0.0234 0.122 Uiso calc R 1 . . H
H16B 0.8710 0.7247 0.0557 0.122 Uiso calc R 1 . . H
H16C 0.9227 0.6479 0.1411 0.122 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
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'
Rh Rh -1.1178 0.9187 '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
C6 Rh1 O1 177.45(14) y
C6 Rh1 O2 94.38(13) y
O1 Rh1 O2 88.03(10) y
C6 Rh1 P1 89.44(12) y
O1 Rh1 P1 88.15(7) y
O2 Rh1 P1 176.15(7) y
C10 P1 C7 104.8(2) y
C10 P1 C13 104.03(16) y
C7 P1 C13 103.08(17) y
C10 P1 Rh1 111.84(13) y
C7 P1 Rh1 117.82(11) y
C13 P1 Rh1 113.89(12) ?
C1 O1 Rh1 128.1(2) ?
C3 O2 Rh1 126.5(2) ?
O1 C1 C2 125.0(3) ?
O1 C1 C5 114.9(3) ?
C2 C1 C5 120.1(3) ?
C1 C2 C3 126.9(3) ?
C1 C2 H2A 116.5 ?
C3 C2 H2A 116.5 ?
O2 C3 C2 125.4(3) ?
O2 C3 C4 115.6(3) ?
C2 C3 C4 119.0(3) ?
C3 C4 H4A 109.5 ?
C3 C4 H4B 109.5 ?
H4A C4 H4B 109.5 ?
C3 C4 H4C 109.5 ?
H4A C4 H4C 109.5 ?
H4B C4 H4C 109.5 ?
C1 C5 H5A 109.5 ?
C1 C5 H5B 109.5 ?
H5A C5 H5B 109.5 ?
C1 C5 H5C 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
O3 C6 Rh1 178.8(3) y
C8 C7 P1 115.5(3) y
C8 C7 H7A 108.4 ?
P1 C7 H7A 108.4 ?
C8 C7 H7B 108.4 ?
P1 C7 H7B 108.4 ?
H7A C7 H7B 107.5 ?
C9 C8 C7 125.3(5) y
C9 C8 H8A 117.3 ?
C7 C8 H8A 117.3 ?
C8 C9 H9A 120.0 ?
C8 C9 H9B 120.0 ?
H9A C9 H9B 120.0 ?
C11 C10 P1 115.2(2) y
C11 C10 H10A 108.5 ?
P1 C10 H10A 108.5 ?
C11 C10 H10B 108.5 ?
P1 C10 H10B 108.5 ?
H10A C10 H10B 107.5 ?
C12 C11 C10 126.0(4) y
C12 C11 H11A 117.0 ?
C10 C11 H11A 117.0 ?
C11 C12 H12A 120.0 ?
C11 C12 H12B 120.0 ?
H12A C12 H12B 120.0 ?
C16 C13 C15 109.3(3) ?
C16 C13 C14 109.4(4) ?
C15 C13 C14 110.0(4) ?
C16 C13 P1 107.4(3) ?
C15 C13 P1 112.6(3) ?
C14 C13 P1 107.9(2) ?
C13 C14 H14A 109.5 ?
C13 C14 H14B 109.5 ?
H14A C14 H14B 109.5 ?
C13 C14 H14C 109.5 ?
H14A C14 H14C 109.5 ?
H14B C14 H14C 109.5 ?
C13 C15 H15A 109.5 ?
C13 C15 H15B 109.5 ?
H15A C15 H15B 109.5 ?
C13 C15 H15C 109.5 ?
H15A C15 H15C 109.5 ?
H15B C15 H15C 109.5 ?
C13 C16 H16A 109.5 ?
C13 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
C13 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
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
Rh1 C6 . 1.797(4) y
Rh1 O1 . 2.036(2) y
Rh1 O2 . 2.082(2) y
Rh1 P1 . 2.2387(8) y
P1 C10 . 1.826(3) y
P1 C7 . 1.834(3) y
P1 C13 . 1.869(3) y
O1 C1 . 1.272(4) y
O2 C3 . 1.264(4) y
O3 C6 . 1.141(4) y
C1 C2 . 1.377(5) y
C1 C5 . 1.490(5) y
C2 C3 . 1.395(5) y
C2 H2A . 0.930 ?
C3 C4 . 1.500(5) y
C4 H4A . 0.960 ?
C4 H4B . 0.960 ?
C4 H4C . 0.960 ?
C5 H5A . 0.960 ?
C5 H5B . 0.960 ?
C5 H5C . 0.960 ?
C7 C8 . 1.493(5) y
C7 H7A . 0.970 ?
C7 H7B . 0.970 ?
C8 C9 . 1.267(7) y
C8 H8A . 0.930 ?
C9 H9A . 0.930 ?
C9 H9B . 0.930 ?
C10 C11 . 1.487(5) y
C10 H10A . 0.970 ?
C10 H10B . 0.970 ?
C11 C12 . 1.270(6) y
C11 H11A . 0.930 ?
C12 H12A . 0.930 ?
C12 H12B . 0.930 ?
C13 C16 . 1.528(5) y
C13 C15 . 1.529(5) y
C13 C14 . 1.536(5) y
C14 H14A . 0.960 ?
C14 H14B . 0.960 ?
C14 H14C . 0.960 ?
C15 H15A . 0.960 ?
C15 H15B . 0.960 ?
C15 H15C . 0.960 ?
C16 H16A . 0.960 ?
C16 H16B . 0.960 ?
C16 H16C . 0.960 ?
