#------------------------------------------------------------------------------
#$Date: 2023-02-09 10:41:28 +0200 (Thu, 09 Feb 2023) $
#$Revision: 280836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/67/8106733.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_8106733
loop_
_publ_author_name
'Manicum, Amanda-Lee'
'Alexander, Orbett'
'Schutte-Smith, Marietjie'
'Visser, Hendrik G.'
'Roodt, Andreas'
_publ_section_title
;
 Crystal structure of fac-(acetylacetonato-κ2
 O,O′)tricarbonyl(benzyldiphenylphosphine-\kP)rhenium(I),
 C27H24O5PRe
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              957
_journal_page_last               959
_journal_paper_doi               10.1515/ncrs-2017-0097
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C27 H24 O5 P Re'
_chemical_formula_sum            'C27 H24 O5 P Re'
_chemical_formula_weight         645.64
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                89.688(6)
_cell_angle_beta                 70.083(6)
_cell_angle_gamma                76.315(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0305(17)
_cell_length_b                   12.084(2)
_cell_length_c                   12.403(2)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      3.77
_cell_volume                     1232.2(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND 3.0c (Brandenburg & Putz, 2005)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program. J. Appl. 
Cryst.(2009).42,339-341
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.(2008). A64,112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6098
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         1.740
_exptl_absorpt_coefficient_mu    5.031
_exptl_absorpt_correction_T_max  0.566
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0151P)²+1.6392P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0432
_reflns_number_gt                5829
_reflns_number_total             6098
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2017-0097_suppl.cif
_cod_data_source_block           16oam4_0m
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8106733
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.19351(2) 0.29170(2) 0.12807(2) 0.01370(3) Uani 1 1 d . . . . .
P1 P 0.18998(7) 0.20541(5) 0.30979(5) 0.01253(11) Uani 1 1 d . . . . .
O1 O -0.1769(2) 0.38212(16) 0.22543(17) 0.0255(4) Uani 1 1 d . . . . .
O2 O 0.1399(3) 0.07837(17) 0.02860(17) 0.0271(4) Uani 1 1 d . . . . .
O3 O 0.1887(3) 0.3977(2) -0.0991(2) 0.0434(6) Uani 1 1 d . . . . .
O5 O 0.2380(2) 0.43764(15) 0.19616(16) 0.0196(4) Uani 1 1 d . . . . .
O4 O 0.4521(2) 0.22899(15) 0.06561(15) 0.0187(3) Uani 1 1 d . . . . .
C24 C -0.1320(3) -0.0925(2) 0.2441(2) 0.0246(5) Uani 1 1 d . . . . .
H24 H -0.1588 -0.1519 0.2103 0.029 Uiso 1 1 calc R U . . .
C25 C -0.0147(3) -0.1183(2) 0.2949(2) 0.0232(5) Uani 1 1 d . . . . .
H25 H 0.0388 -0.1958 0.2966 0.028 Uiso 1 1 calc R U . . .
C26 C 0.0252(3) -0.0316(2) 0.3435(2) 0.0186(5) Uani 1 1 d . . . . .
H26 H 0.1055 -0.0505 0.3786 0.022 Uiso 1 1 calc R U . . .
C23 C -0.2101(3) 0.0208(2) 0.2428(2) 0.0253(6) Uani 1 1 d . . . . .
H23 H -0.2918 0.0391 0.2089 0.030 Uiso 1 1 calc R U . . .
C16 C 0.1095(3) 0.3554(2) 0.5081(2) 0.0219(5) Uani 1 1 d . . . . .
H16 H -0.0008 0.3555 0.5227 0.026 Uiso 1 1 calc R U . . .
C21 C -0.0506(3) 0.0828(2) 0.3417(2) 0.0162(4) Uani 1 1 d . . . . .
C22 C -0.1693(3) 0.1078(2) 0.2908(2) 0.0210(5) Uani 1 1 d . . . . .
H22 H -0.2230 0.1851 0.2888 0.025 Uiso 1 1 calc R U . . .
C27 C -0.0077(3) 0.1770(2) 0.3957(2) 0.0171(5) Uani 1 1 d . . . . .
H27A H -0.0050 0.1562 0.4725 0.021 Uiso 1 1 calc R U . . .
H27B H -0.0944 0.2481 0.4072 0.021 Uiso 1 1 calc R U . . .
C35 C 0.4843(3) -0.1168(2) 0.2006(2) 0.0199(5) Uani 1 1 d . . . . .
H35 H 0.5311 -0.1651 0.1312 0.024 Uiso 1 1 calc R U . . .
C36 C 0.3999(3) -0.0040(2) 0.2010(2) 0.0157(4) Uani 1 1 d . . . . .
H36 H 0.3902 0.0246 0.1316 0.019 Uiso 1 1 calc R U . . .
C14 C 0.3090(4) 0.4196(2) 0.5622(2) 0.0259(6) Uani 1 1 d . . . . .
H14 H 0.3360 0.4617 0.6142 0.031 Uiso 1 1 calc R U . . .
C34 C 0.4997(3) -0.1583(2) 0.3018(2) 0.0201(5) Uani 1 1 d . . . . .
H34 H 0.5554 -0.2356 0.3018 0.024 Uiso 1 1 calc R U . . .
C31 C 0.3297(3) 0.06701(19) 0.3030(2) 0.0140(4) Uani 1 1 d . . . . .
C32 C 0.3492(3) 0.0252(2) 0.4040(2) 0.0169(5) Uani 1 1 d . . . . .
H32 H 0.3044 0.0738 0.4732 0.020 Uiso 1 1 calc R U . . .
C33 C 0.4339(3) -0.0871(2) 0.4034(2) 0.0187(5) Uani 1 1 d . . . . .
H33 H 0.4468 -0.1153 0.4722 0.022 Uiso 1 1 calc R U . . .
C5 C 0.5586(3) 0.2839(2) 0.0614(2) 0.0185(5) Uani 1 1 d . . . . .
C11 C 0.2311(3) 0.2923(2) 0.4111(2) 0.0160(4) Uani 1 1 d . . . . .
C12 C 0.3919(3) 0.2954(2) 0.3892(2) 0.0196(5) Uani 1 1 d . . . . .
H12 H 0.4755 0.2538 0.3228 0.023 Uiso 1 1 calc R U . . .
C8 C 0.3628(4) 0.5744(2) 0.2351(3) 0.0324(7) Uani 1 1 d . . . . .
H8A H 0.2486 0.6115 0.2786 0.049 Uiso 1 1 calc R U . . .
H8B H 0.4086 0.6240 0.1769 0.049 Uiso 1 1 calc R U . . .
H8C H 0.4241 0.5606 0.2876 0.049 Uiso 1 1 calc R U . . .
C7 C 0.3735(3) 0.4622(2) 0.1767(2) 0.0205(5) Uani 1 1 d . . . . .
C6 C 0.5261(3) 0.3947(2) 0.1098(2) 0.0220(5) Uani 1 1 d . . . . .
H6 H 0.6162 0.4274 0.0959 0.026 Uiso 1 1 calc R U . . .
C4 C 0.7328(3) 0.2191(3) -0.0006(3) 0.0272(6) Uani 1 1 d . . . . .
H4A H 0.7354 0.1430 -0.0294 0.041 Uiso 1 1 calc R U . . .
H4B H 0.7930 0.2113 0.0526 0.041 Uiso 1 1 calc R U . . .
H4C H 0.7831 0.2607 -0.0654 0.041 Uiso 1 1 calc R U . . .
C3 C 0.1949(4) 0.3613(2) -0.0148(2) 0.0254(6) Uani 1 1 d . . . . .
C15 C 0.1486(4) 0.4185(2) 0.5836(2) 0.0271(6) Uani 1 1 d . . . . .
H15 H 0.0651 0.4606 0.6498 0.033 Uiso 1 1 calc R U . . .
C2 C 0.1598(3) 0.1578(2) 0.0673(2) 0.0180(5) Uani 1 1 d . . . . .
C1 C -0.0364(3) 0.3486(2) 0.1884(2) 0.0183(5) Uani 1 1 d . . . . .
C13 C 0.4306(3) 0.3592(2) 0.4645(2) 0.0244(5) Uani 1 1 d . . . . .
H13 H 0.5404 0.3614 0.4489 0.029 Uiso 1 1 calc R U . . .
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'
Re Re -1.018 7.231 '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
C1 Re1 C2 87.68(10) . .
C1 Re1 C3 88.95(11) . .
C2 Re1 C3 88.50(11) . .
C1 Re1 O4 178.17(8) . .
C2 Re1 O4 93.49(9) . .
C3 Re1 O4 92.49(10) . .
C1 Re1 O5 93.88(9) . .
C2 Re1 O5 178.21(8) . .
C3 Re1 O5 92.40(10) . .
O4 Re1 O5 84.93(7) . .
C1 Re1 P1 90.68(7) . .
C2 Re1 P1 91.88(7) . .
C3 Re1 P1 179.46(9) . .
O4 Re1 P1 87.87(5) . .
O5 Re1 P1 87.23(5) . .
C31 P1 C11 102.29(11) . .
C31 P1 C27 101.33(11) . .
C11 P1 C27 103.39(11) . .
C31 P1 Re1 118.68(8) . .
C11 P1 Re1 114.94(8) . .
C27 P1 Re1 114.09(8) . .
C7 O5 Re1 127.91(16) . .
C5 O4 Re1 127.94(16) . .
C25 C24 C23 119.4(2) . .
C25 C24 H24 120.3 . .
C23 C24 H24 120.3 . .
C24 C25 C26 120.3(3) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C25 C26 C21 121.0(2) . .
C25 C26 H26 119.5 . .
C21 C26 H26 119.5 . .
C24 C23 C22 120.3(2) . .
C24 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C15 C16 C11 120.6(2) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C26 C21 C22 118.2(2) . .
C26 C21 C27 120.8(2) . .
C22 C21 C27 121.0(2) . .
C23 C22 C21 120.8(3) . .
C23 C22 H22 119.6 . .
C21 C22 H22 119.6 . .
C21 C27 P1 114.06(16) . .
C21 C27 H27A 108.7 . .
P1 C27 H27A 108.7 . .
C21 C27 H27B 108.7 . .
P1 C27 H27B 108.7 . .
H27A C27 H27B 107.6 . .
C34 C35 C36 119.9(2) . .
C34 C35 H35 120.0 . .
C36 C35 H35 120.0 . .
C35 C36 C31 120.3(2) . .
C35 C36 H36 119.9 . .
C31 C36 H36 119.9 . .
C15 C14 C13 119.9(2) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C35 C34 C33 120.3(2) . .
C35 C34 H34 119.9 . .
C33 C34 H34 119.9 . .
C36 C31 C32 119.4(2) . .
C36 C31 P1 120.35(18) . .
C32 C31 P1 119.67(18) . .
C33 C32 C31 120.3(2) . .
C33 C32 H32 119.9 . .
C31 C32 H32 119.9 . .
C32 C33 C34 119.9(2) . .
C32 C33 H33 120.1 . .
C34 C33 H33 120.1 . .
O4 C5 C6 125.6(2) . .
O4 C5 C4 115.1(2) . .
C6 C5 C4 119.3(2) . .
C12 C11 C16 119.0(2) . .
C12 C11 P1 117.84(18) . .
C16 C11 P1 123.12(19) . .
C11 C12 C13 120.3(2) . .
C11 C12 H12 119.9 . .
C13 C12 H12 119.9 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O5 C7 C6 126.1(2) . .
O5 C7 C8 114.8(2) . .
C6 C7 C8 119.0(2) . .
C5 C6 C7 126.0(2) . .
C5 C6 H6 117.0 . .
C7 C6 H6 117.0 . .
C5 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C5 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O3 C3 Re1 175.3(3) . .
C14 C15 C16 120.0(2) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
O2 C2 Re1 178.5(2) . .
O1 C1 Re1 179.3(2) . .
C14 C13 C12 120.2(2) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C1 1.902(3) .
Re1 C2 1.919(3) .
Re1 C3 1.954(3) .
Re1 O4 2.1362(18) .
Re1 O5 2.1369(17) .
Re1 P1 2.4718(7) .
P1 C31 1.824(2) .
P1 C11 1.826(2) .
P1 C27 1.852(2) .
O1 C1 1.160(3) .
O2 C2 1.152(3) .
O3 C3 1.147(3) .
O5 C7 1.271(3) .
O4 C5 1.279(3) .
C24 C25 1.384(4) .
C24 C23 1.387(4) .
C24 H24 0.9500 .
C25 C26 1.387(4) .
C25 H25 0.9500 .
C26 C21 1.394(4) .
C26 H26 0.9500 .
C23 C22 1.390(4) .
C23 H23 0.9500 .
C16 C15 1.394(4) .
C16 C11 1.396(3) .
C16 H16 0.9500 .
C21 C22 1.395(3) .
C21 C27 1.513(3) .
C22 H22 0.9500 .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C35 C34 1.388(4) .
C35 C36 1.394(3) .
C35 H35 0.9500 .
C36 C31 1.395(3) .
C36 H36 0.9500 .
C14 C15 1.385(4) .
C14 C13 1.390(4) .
C14 H14 0.9500 .
C34 C33 1.393(4) .
C34 H34 0.9500 .
C31 C32 1.399(3) .
C32 C33 1.390(3) .
C32 H32 0.9500 .
C33 H33 0.9500 .
C5 C6 1.394(4) .
C5 C4 1.510(4) .
C11 C12 1.393(3) .
C12 C13 1.395(3) .
C12 H12 0.9500 .
C8 C7 1.507(4) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C7 C6 1.396(4) .
C6 H6 0.9500 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C15 H15 0.9500 .
C13 H13 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C23 C24 C25 C26 -0.4(4) . . . .
C24 C25 C26 C21 -0.4(4) . . . .
C25 C24 C23 C22 0.9(4) . . . .
C25 C26 C21 C22 0.7(4) . . . .
C25 C26 C21 C27 179.5(2) . . . .
C24 C23 C22 C21 -0.5(4) . . . .
C26 C21 C22 C23 -0.3(4) . . . .
C27 C21 C22 C23 -179.0(2) . . . .
C26 C21 C27 P1 75.5(3) . . . .
C22 C21 C27 P1 -105.8(2) . . . .
C31 P1 C27 C21 -60.01(19) . . . .
C11 P1 C27 C21 -165.72(17) . . . .
Re1 P1 C27 C21 68.73(19) . . . .
C34 C35 C36 C31 -0.6(4) . . . .
C36 C35 C34 C33 -1.2(4) . . . .
C35 C36 C31 C32 2.1(3) . . . .
C35 C36 C31 P1 -169.19(18) . . . .
C11 P1 C31 C36 -146.91(19) . . . .
C27 P1 C31 C36 106.5(2) . . . .
Re1 P1 C31 C36 -19.2(2) . . . .
C11 P1 C31 C32 41.8(2) . . . .
C27 P1 C31 C32 -64.7(2) . . . .
Re1 P1 C31 C32 169.53(16) . . . .
C36 C31 C32 C33 -1.8(3) . . . .
P1 C31 C32 C33 169.48(18) . . . .
C31 C32 C33 C34 0.1(4) . . . .
C35 C34 C33 C32 1.4(4) . . . .
Re1 O4 C5 C6 7.9(4) . . . .
Re1 O4 C5 C4 -172.99(16) . . . .
C15 C16 C11 C12 -1.6(4) . . . .
C15 C16 C11 P1 178.8(2) . . . .
C31 P1 C11 C12 52.9(2) . . . .
C27 P1 C11 C12 157.84(19) . . . .
Re1 P1 C11 C12 -77.2(2) . . . .
C31 P1 C11 C16 -127.5(2) . . . .
C27 P1 C11 C16 -22.5(2) . . . .
Re1 P1 C11 C16 102.5(2) . . . .
C16 C11 C12 C13 1.1(4) . . . .
P1 C11 C12 C13 -179.2(2) . . . .
Re1 O5 C7 C6 -3.5(4) . . . .
Re1 O5 C7 C8 177.82(18) . . . .
O4 C5 C6 C7 4.1(4) . . . .
C4 C5 C6 C7 -175.0(3) . . . .
O5 C7 C6 C5 -6.5(4) . . . .
C8 C7 C6 C5 172.1(3) . . . .
C13 C14 C15 C16 0.9(4) . . . .
C11 C16 C15 C14 0.6(4) . . . .
C15 C14 C13 C12 -1.4(4) . . . .
C11 C12 C13 C14 0.4(4) . . . .
