#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:10:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178551 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/58/4065864.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_4065864
loop_
_publ_author_name
'Christiansen, Andrea'
'Selent, Detlef'
'Spannenberg, Anke'
'Baumann, Wolfgang'
'Franke, Robert'
'Börner, Armin'
_publ_section_title
;
 Reaction of Secondary Phosphine Oxides with Rhodium(I)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3139
_journal_paper_doi               10.1021/om100171p
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C32 H32 B F2 O2 P2 Rh'
_chemical_formula_weight         662.24
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.546(3)
_cell_length_b                   17.317(4)
_cell_length_c                   13.706(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    200(2)
_cell_volume                     2924.6(12)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE-IPDS I'
_diffrn_measurement_method       'rotation method'
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10470
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5630
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0198P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                4330
_reflns_number_total             5630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100171p_si_001.cif
_cod_data_source_block           11
_cod_original_cell_volume        2924.6(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065864
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_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
B1 B 0.6950(2) 0.23026(15) 0.61380(19) 0.0230(6) Uani 1 1 d .
C1 C 0.7264(2) 0.14874(14) 1.00778(17) 0.0253(6) Uani 1 1 d .
C2 C 0.8146(2) 0.12805(15) 1.09475(17) 0.0318(6) Uani 1 1 d .
H2A H 0.8020 0.0748 1.1162 0.038 Uiso 1 1 calc R
H2B H 0.8094 0.1631 1.1508 0.038 Uiso 1 1 calc R
C3 C 0.9303(2) 0.13313(15) 1.07237(19) 0.0334(6) Uani 1 1 d .
H3A H 0.9557 0.1872 1.0821 0.040 Uiso 1 1 calc R
H3B H 0.9790 0.1007 1.1210 0.040 Uiso 1 1 calc R
C4 C 0.9400(2) 0.10799(14) 0.96934(18) 0.0259(6) Uani 1 1 d .
C5 C 0.8880(2) 0.04755(13) 0.91721(19) 0.0247(6) Uani 1 1 d .
C6 C 0.8162(2) -0.00934(13) 0.95830(18) 0.0289(6) Uani 1 1 d .
H6A H 0.8400 -0.0126 1.0313 0.035 Uiso 1 1 calc R
H6B H 0.8253 -0.0611 0.9303 0.035 Uiso 1 1 calc R
C7 C 0.6962(2) 0.01265(14) 0.9349(2) 0.0327(6) Uani 1 1 d .
H7A H 0.6644 -0.0068 0.8678 0.039 Uiso 1 1 calc R
H7B H 0.6586 -0.0137 0.9829 0.039 Uiso 1 1 calc R
C8 C 0.6744(2) 0.09833(14) 0.93836(19) 0.0266(6) Uani 1 1 d .
C9 C 0.75068(19) 0.34992(12) 0.86629(17) 0.0218(5) Uani 1 1 d .
C10 C 0.7534(2) 0.41512(13) 0.80800(19) 0.0314(6) Uani 1 1 d .
H10A H 0.7182 0.4145 0.7403 0.038 Uiso 1 1 calc R
C11 C 0.8071(2) 0.48090(15) 0.8478(2) 0.0395(7) Uani 1 1 d D
H11A H 0.8085 0.5253 0.8074 0.047 Uiso 1 1 calc R
C12 C 0.8581(2) 0.48232(14) 0.94518(17) 0.0412(7) Uani 1 1 d D
H12A H 0.8954 0.5276 0.9720 0.049 Uiso 1 1 calc R
C13 C 0.8557(3) 0.41874(16) 1.0043(2) 0.0486(8) Uani 1 1 d D
H13A H 0.8902 0.4202 1.0722 0.058 Uiso 1 1 calc R
C14 C 0.8027(2) 0.35214(15) 0.96477(19) 0.0377(7) Uani 1 1 d .
H14A H 0.8022 0.3078 1.0056 0.045 Uiso 1 1 calc R
C15 C 0.55188(19) 0.25945(12) 0.83170(17) 0.0216(5) Uani 1 1 d .
C16 C 0.4752(2) 0.21742(14) 0.76591(19) 0.0290(6) Uani 1 1 d .
H16A H 0.4957 0.1924 0.7106 0.035 Uiso 1 1 calc R
C17 C 0.3692(2) 0.21195(16) 0.7807(2) 0.0386(7) Uani 1 1 d .
H17A H 0.3172 0.1835 0.7352 0.046 Uiso 1 1 calc R
C18 C 0.3389(2) 0.24785(17) 0.8615(2) 0.0418(7) Uani 1 1 d .
H18A H 0.2663 0.2439 0.8717 0.050 Uiso 1 1 calc R
C19 C 0.4140(2) 0.28911(15) 0.9267(2) 0.0380(7) Uani 1 1 d .
H19A H 0.3929 0.3139 0.9820 0.046 Uiso 1 1 calc R
C20 C 0.5205(2) 0.29508(14) 0.91302(18) 0.0291(6) Uani 1 1 d .
H20A H 0.5719 0.3234 0.9590 0.035 Uiso 1 1 calc R
C21 C 0.97924(19) 0.11695(12) 0.71350(17) 0.0216(5) Uani 1 1 d .
C22 C 0.9438(2) 0.05910(14) 0.64439(19) 0.0320(6) Uani 1 1 d .
H22A H 0.8717 0.0600 0.6074 0.038 Uiso 1 1 calc R
C23 C 1.0140(3) 0.00014(15) 0.6296(2) 0.0431(7) Uani 1 1 d D
H23A H 0.9893 -0.0396 0.5831 0.052 Uiso 1 1 calc R
C24 C 1.1189(2) -0.00131(15) 0.68161(19) 0.0432(7) Uani 1 1 d D
H24A H 1.1664 -0.0418 0.6706 0.052 Uiso 1 1 calc R
C25 C 1.1553(2) 0.05571(14) 0.7495(2) 0.0381(7) Uani 1 1 d D
H25A H 1.2279 0.0547 0.7854 0.046 Uiso 1 1 calc R
C26 C 1.0855(2) 0.11489(14) 0.7657(2) 0.0312(6) Uani 1 1 d .
H26A H 1.1107 0.1542 0.8128 0.037 Uiso 1 1 calc R
C27 C 0.96268(19) 0.27780(13) 0.75022(17) 0.0210(5) Uani 1 1 d .
C28 C 0.9686(2) 0.32069(13) 0.66552(19) 0.0304(6) Uani 1 1 d .
H28A H 0.9290 0.3050 0.6027 0.036 Uiso 1 1 calc R
C29 C 1.0327(2) 0.38653(15) 0.6733(2) 0.0405(7) Uani 1 1 d .
H29A H 1.0372 0.4157 0.6155 0.049 Uiso 1 1 calc R
C30 C 1.0896(2) 0.40961(15) 0.7641(2) 0.0417(7) Uani 1 1 d .
H30A H 1.1326 0.4551 0.7688 0.050 Uiso 1 1 calc R
C31 C 1.0850(2) 0.36750(15) 0.8484(2) 0.0390(7) Uani 1 1 d .
H31A H 1.1258 0.3831 0.9108 0.047 Uiso 1 1 calc R
C32 C 1.0200(2) 0.30185(14) 0.84154(19) 0.0290(6) Uani 1 1 d .
H32A H 1.0149 0.2734 0.8998 0.035 Uiso 1 1 calc R
F1 F 0.61805(12) 0.17176(8) 0.59530(11) 0.0380(4) Uani 1 1 d .
F2 F 0.68865(12) 0.27638(8) 0.53043(9) 0.0359(4) Uani 1 1 d .
O1 O 0.67368(12) 0.27997(8) 0.69488(10) 0.0199(4) Uani 1 1 d .
O2 O 0.80386(13) 0.19479(9) 0.63592(11) 0.0240(4) Uani 1 1 d .
P1 P 0.69039(5) 0.26115(3) 0.80956(4) 0.01811(13) Uani 1 1 d .
P2 P 0.88296(5) 0.18925(3) 0.73994(4) 0.01914(13) Uani 1 1 d .
Rh1 Rh 0.797079(15) 0.160402(10) 0.867863(13) 0.01858(6) Uani 1 1 d .
H1 H 0.692(2) 0.1938(14) 1.0158(17) 0.025(7) Uiso 1 1 d .
H4 H 0.998(2) 0.1297(14) 0.9500(18) 0.031(7) Uiso 1 1 d .
H5 H 0.9106(18) 0.0317(12) 0.8582(16) 0.017(6) Uiso 1 1 d .
H8 H 0.605(2) 0.1127(13) 0.9012(17) 0.020(6) Uiso 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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
F2 B1 F1 109.9(2)
F2 B1 O1 107.21(19)
F1 B1 O1 110.27(19)
F2 B1 O2 108.47(19)
F1 B1 O2 108.56(19)
O1 B1 O2 112.41(19)
C8 C1 C2 125.6(2)
C8 C1 Rh1 71.26(13)
C2 C1 Rh1 110.11(16)
C1 C2 C3 114.0(2)
C4 C3 C2 114.6(2)
C5 C4 C3 126.8(2)
C5 C4 Rh1 74.82(15)
C3 C4 Rh1 105.58(16)
C4 C5 C6 124.4(2)
C4 C5 Rh1 70.32(14)
C6 C5 Rh1 111.42(16)
C5 C6 C7 113.07(19)
C8 C7 C6 114.5(2)
C1 C8 C7 125.8(3)
C1 C8 Rh1 73.53(14)
C7 C8 Rh1 108.33(16)
C14 C9 C10 118.7(2)
C14 C9 P1 121.41(18)
C10 C9 P1 119.61(18)
C11 C10 C9 120.4(2)
C12 C11 C10 120.3(2)
C11 C12 C13 120.3(3)
C12 C13 C14 119.9(2)
C9 C14 C13 120.4(2)
C16 C15 C20 118.9(2)
C16 C15 P1 117.73(17)
C20 C15 P1 123.28(19)
C17 C16 C15 120.4(2)
C18 C17 C16 120.1(3)
C19 C18 C17 119.8(3)
C18 C19 C20 120.7(2)
C19 C20 C15 120.0(3)
C26 C21 C22 119.0(2)
C26 C21 P2 121.51(18)
C22 C21 P2 119.37(19)
C23 C22 C21 119.9(3)
C24 C23 C22 120.7(2)
C23 C24 C25 120.1(2)
C24 C25 C26 119.8(3)
C21 C26 C25 120.5(2)
C32 C27 C28 119.5(2)
C32 C27 P2 120.48(18)
C28 C27 P2 119.96(18)
C29 C28 C27 119.7(3)
C30 C29 C28 120.2(3)
C29 C30 C31 120.7(3)
C30 C31 C32 119.5(3)
C27 C32 C31 120.3(2)
B1 O1 P1 128.49(14)
B1 O2 P2 127.64(14)
O1 P1 C15 102.53(10)
O1 P1 C9 102.55(9)
C15 P1 C9 105.98(10)
O1 P1 Rh1 118.14(6)
C15 P1 Rh1 116.79(7)
C9 P1 Rh1 109.32(8)
O2 P2 C27 105.15(10)
O2 P2 C21 100.93(10)
C27 P2 C21 102.64(10)
O2 P2 Rh1 113.58(6)
C27 P2 Rh1 117.20(7)
C21 P2 Rh1 115.42(7)
C8 Rh1 C4 94.14(10)
C8 Rh1 P1 96.55(7)
C4 Rh1 P1 152.33(7)
C8 Rh1 C1 35.21(9)
C4 Rh1 C1 80.42(9)
P1 Rh1 C1 93.92(7)
C8 Rh1 P2 154.10(7)
C4 Rh1 P2 97.32(7)
P1 Rh1 P2 83.84(3)
C1 Rh1 P2 170.56(7)
C8 Rh1 C5 78.96(9)
C4 Rh1 C5 34.87(9)
P1 Rh1 C5 172.58(7)
C1 Rh1 C5 85.81(9)
P2 Rh1 C5 97.60(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
B1 F2 1.384(3)
B1 F1 1.389(3)
B1 O1 1.469(3)
B1 O2 1.476(3)
C1 C8 1.364(4)
C1 C2 1.509(4)
C1 Rh1 2.268(2)
C2 C3 1.541(4)
C3 C4 1.504(3)
C4 C5 1.362(4)
C4 Rh1 2.244(3)
C5 C6 1.514(3)
C5 Rh1 2.300(2)
C6 C7 1.527(4)
C7 C8 1.511(3)
C8 Rh1 2.240(2)
C9 C14 1.385(3)
C9 C10 1.387(3)
C9 P1 1.822(2)
C10 C11 1.382(4)
C11 C12 1.368(3)
C12 C13 1.370(3)
C13 C14 1.389(4)
C15 C16 1.394(3)
C15 C20 1.394(3)
C15 P1 1.820(2)
C16 C17 1.386(3)
C17 C18 1.384(4)
C18 C19 1.372(4)
C19 C20 1.387(4)
C21 C26 1.389(4)
C21 C22 1.393(3)
C21 P2 1.823(2)
C22 C23 1.388(4)
C23 C24 1.374(3)
C24 C25 1.375(3)
C25 C26 1.393(3)
C27 C32 1.385(3)
C27 C28 1.392(3)
C27 P2 1.822(2)
C28 C29 1.388(4)
C29 C30 1.372(4)
C30 C31 1.378(4)
C31 C32 1.392(4)
O1 P1 1.5800(15)
O2 P2 1.5794(17)
P1 Rh1 2.2520(7)
P2 Rh1 2.2793(8)
