#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/12/7051278.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_7051278
loop_
_publ_author_name
'Pierre Braunstein'
'Yves Chauvin'
'Jean Fischer'
'Hélène Olivier'
'Carsten Strohmann'
'Dawn V. Toronto'
_publ_section_title
;
 Oxidative addition of iodine, iodomethane and iodobenzene to the
 rhodium phosphino enolate complex[Rh{Ph2PCHC(O)Ph}(CO)(PPh3)] and
 carbon monoxide insertion into the resulting Rh--carbon bond of
 [Rh{Ph2PCHC(O)Ph}Me(I)(CO)(PPh3)]
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              437
_journal_page_last               445
_journal_paper_doi               10.1039/b000961j
_journal_volume                  24
_journal_year                    2000
_chemical_formula_sum            'C41 H36 O2.5 P2 Rh'
_chemical_formula_weight         733.55
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.864(3)
_cell_length_b                   8.859(2)
_cell_length_c                   29.696(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     3577.0(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Siemens Stoe AED2'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            25660
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    'riding model, H3 isotropic'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_obs          0.0365
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0432P)²+2.5140P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1066
_refine_ls_wR_factor_obs         0.0916
_reflns_number_observed          5690
_reflns_number_total             6624
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000961j.txt
_cod_data_source_block           shelx834
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'monoklinic' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+2.5140P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+2.5140P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3577.0(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C41 H36 O2.50 P2 Rh'
_cod_database_code               7051278
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Rh Rh 0.463344(15) 0.12482(3) 0.137712(7) 0.04333(8) Uani 1 d . .
P1 P 0.60998(5) 0.02939(8) 0.11961(2) 0.0408(2) Uani 1 d . .
P2 P 0.33173(5) 0.20505(9) 0.16678(3) 0.0479(2) Uani 1 d . .
O1 O 0.51175(14) 0.0520(3) 0.20413(7) 0.0542(5) Uani 1 d . .
O2 O 0.3698(2) 0.2433(4) 0.04675(9) 0.0950(10) Uani 1 d . .
C1 C 0.4099(2) 0.1955(4) 0.08143(12) 0.0604(8) Uani 1 d . .
C2 C 0.4568(2) 0.0792(3) 0.23485(10) 0.0496(7) Uani 1 d . .
C3 C 0.3651(2) 0.1409(4) 0.22381(11) 0.0569(8) Uani 1 d . .
H3 H 0.3283(23) 0.1565(34) 0.2455(12) 0.052(9) Uiso 1 d . .
C4 C 0.5062(2) 0.0478(4) 0.28319(10) 0.0532(7) Uani 1 d . .
C5 C 0.6039(3) 0.0073(5) 0.29322(13) 0.0734(10) Uani 1 d . .
H5 H 0.6367(3) -0.0108(5) 0.26925(13) 0.088 Uiso 1 calc R .
C6 C 0.6548(3) -0.0072(6) 0.3380(2) 0.0871(13) Uani 1 d . .
H6 H 0.7210(3) -0.0333(6) 0.3439(2) 0.105 Uiso 1 calc R .
C7 C 0.6081(4) 0.0166(6) 0.37319(14) 0.0913(13) Uani 1 d . .
H7 H 0.6419(4) 0.0060(6) 0.40332(14) 0.110 Uiso 1 calc R .
C8 C 0.5102(4) 0.0567(8) 0.3643(2) 0.117(2) Uani 1 d . .
H8 H 0.4780(4) 0.0732(8) 0.3886(2) 0.141 Uiso 1 calc R .
C9 C 0.4598(3) 0.0723(6) 0.31986(13) 0.0908(14) Uani 1 d . .
H9 H 0.3938(3) 0.0998(6) 0.31433(13) 0.109 Uiso 1 calc R .
C10 C 0.3179(2) 0.4093(4) 0.16941(10) 0.0511(7) Uani 1 d . .
C11 C 0.3626(2) 0.4905(4) 0.20789(12) 0.0646(9) Uani 1 d . .
H11 H 0.3951(2) 0.4391(4) 0.23373(12) 0.077 Uiso 1 calc R .
C12 C 0.3596(3) 0.6469(5) 0.20845(15) 0.0763(10) Uani 1 d . .
H12 H 0.3908(3) 0.6994(5) 0.23436(15) 0.092 Uiso 1 calc R .
C13 C 0.3111(3) 0.7236(5) 0.1711(2) 0.0792(11) Uani 1 d . .
H13 H 0.3093(3) 0.8286(5) 0.1715(2) 0.095 Uiso 1 calc R .
C14 C 0.2649(3) 0.6463(5) 0.13303(15) 0.0802(11) Uani 1 d . .
H14 H 0.2307(3) 0.6990(5) 0.10781(15) 0.096 Uiso 1 calc R .
C15 C 0.2687(3) 0.4892(4) 0.13181(12) 0.0646(9) Uani 1 d . .
H15 H 0.2380(3) 0.4378(4) 0.10560(12) 0.078 Uiso 1 calc R .
C16 C 0.2078(2) 0.1390(4) 0.14244(12) 0.0575(8) Uani 1 d . .
C17 C 0.1918(3) 0.0394(5) 0.1066(2) 0.0774(11) Uani 1 d . .
H17 H 0.2433(3) 0.0115(5) 0.0925(2) 0.093 Uiso 1 calc R .
C18 C 0.0979(3) -0.0203(6) 0.0913(2) 0.111(2) Uani 1 d . .
H18 H 0.0871(3) -0.0882(6) 0.0670(2) 0.133 Uiso 1 calc R .
C19 C 0.0225(3) 0.0198(6) 0.1118(3) 0.119(2) Uani 1 d . .
H19 H -0.0389(3) -0.0244(6) 0.1023(3) 0.143 Uiso 1 calc R .
C20 C 0.0363(3) 0.1254(7) 0.1463(2) 0.112(2) Uani 1 d . .
H20 H -0.0165(3) 0.1572(7) 0.1590(2) 0.135 Uiso 1 calc R .
C21 C 0.1296(3) 0.1841(6) 0.1620(2) 0.0903(13) Uani 1 d . .
H21 H 0.1397(3) 0.2541(6) 0.1858(2) 0.108 Uiso 1 calc R .
C22 C 0.7135(2) 0.0321(3) 0.16825(9) 0.0459(6) Uani 1 d . .
C23 C 0.7216(2) 0.1512(4) 0.19902(12) 0.0639(9) Uani 1 d . .
H23 H 0.6745(2) 0.2273(4) 0.19467(12) 0.077 Uiso 1 calc R .
C24 C 0.7995(3) 0.1580(5) 0.23629(14) 0.0789(11) Uani 1 d . .
H24 H 0.8051(3) 0.2398(5) 0.25629(14) 0.095 Uiso 1 calc R .
C25 C 0.8678(3) 0.0456(5) 0.24371(13) 0.0789(11) Uani 1 d . .
H25 H 0.9190(3) 0.0494(5) 0.26908(13) 0.095 Uiso 1 calc R .
C26 C 0.8606(3) -0.0725(5) 0.2138(2) 0.0791(11) Uani 1 d . .
H26 H 0.9077(3) -0.1487(5) 0.2188(2) 0.095 Uiso 1 calc R .
C27 C 0.7837(2) -0.0804(4) 0.17585(13) 0.0618(8) Uani 1 d . .
H27 H 0.7796(2) -0.1615(4) 0.15566(13) 0.074 Uiso 1 calc R .
C28 C 0.5975(2) -0.1698(3) 0.10399(10) 0.0439(6) Uani 1 d . .
C29 C 0.6349(2) -0.2331(4) 0.06785(11) 0.0570(7) Uani 1 d . .
H29 H 0.6682(2) -0.1730(4) 0.05024(11) 0.068 Uiso 1 calc R .
C30 C 0.6224(3) -0.3855(4) 0.05835(13) 0.0695(9) Uani 1 d . .
H30 H 0.6469(3) -0.4273(4) 0.03416(13) 0.083 Uiso 1 calc R .
C31 C 0.5738(3) -0.4756(4) 0.08443(14) 0.0704(9) Uani 1 d . .
H31 H 0.5663(3) -0.5782(4) 0.07808(14) 0.085 Uiso 1 calc R .
C32 C 0.5363(3) -0.4138(4) 0.11988(14) 0.0703(10) Uani 1 d . .
H32 H 0.5027(3) -0.4743(4) 0.13727(14) 0.084 Uiso 1 calc R .
C33 C 0.5485(2) -0.2625(4) 0.12960(11) 0.0568(7) Uani 1 d . .
H33 H 0.5234(2) -0.2217(4) 0.15377(11) 0.068 Uiso 1 calc R .
C34 C 0.6599(2) 0.1148(3) 0.07275(9) 0.0433(6) Uani 1 d . .
C35 C 0.5989(2) 0.1350(4) 0.03037(11) 0.0558(7) Uani 1 d . .
H35 H 0.5331(2) 0.1071(4) 0.02629(11) 0.067 Uiso 1 calc R .
C36 C 0.6347(3) 0.1964(5) -0.00617(12) 0.0708(10) Uani 1 d . .
H36 H 0.5932(3) 0.2081(5) -0.03460(12) 0.085 Uiso 1 calc R .
C37 C 0.7307(3) 0.2394(5) -0.00028(13) 0.0814(11) Uani 1 d . .
H37 H 0.7548(3) 0.2805(5) -0.02472(13) 0.098 Uiso 1 calc R .
C38 C 0.7917(3) 0.2222(6) 0.04160(14) 0.0860(13) Uani 1 d . .
H38 H 0.8571(3) 0.2524(6) 0.04552(14) 0.103 Uiso 1 calc R .
C39 C 0.7569(2) 0.1600(4) 0.07826(12) 0.0654(9) Uani 1 d . .
H39 H 0.7989(2) 0.1488(4) 0.10658(12) 0.079 Uiso 1 calc R .
C200 C 0.5520(18) 0.1028(38) -0.4982(9) 0.345(22) Uani 1 d . .
H20A H 0.5977(18) 0.0193(38) -0.4912(9) 0.414 Uiso 1 calc R .
H20B H 0.5352(18) 0.1275(38) -0.4689(9) 0.414 Uiso 1 calc R .
C300 C 0.6093(11) 0.2015(27) -0.5001(6) 0.366(16) Uani 1 d . .
H30A H 0.6592(96) 0.1661(84) -0.5158(71) 0.548 Uiso 1 calc R .
H30B H 0.6392(125) 0.2323(182) -0.4696(6) 0.548 Uiso 1 calc R .
H30C H 0.5757(32) 0.2859(102) -0.5164(69) 0.548 Uiso 1 calc R .
O3 O 0.4939(28) 0.0470(55) -0.5116(5) 0.236(16) Uani 0.50 d P .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh O1 174.16(11) . . ?
C1 Rh P2 91.61(10) . . ?
O1 Rh P2 82.54(6) . . ?
C1 Rh P1 97.46(10) . . ?
O1 Rh P1 88.38(6) . . ?
P2 Rh P1 170.92(3) . . ?
C28 P1 C22 103.58(13) . . ?
C28 P1 C34 103.73(13) . . ?
C22 P1 C34 103.88(13) . . ?
C28 P1 Rh 111.19(9) . . ?
C22 P1 Rh 113.20(9) . . ?
C34 P1 Rh 119.65(9) . . ?
C3 P2 C10 106.8(2) . . ?
C3 P2 C16 109.1(2) . . ?
C10 P2 C16 103.67(14) . . ?
C3 P2 Rh 100.61(11) . . ?
C10 P2 Rh 115.12(9) . . ?
C16 P2 Rh 120.77(12) . . ?
C2 O1 Rh 118.7(2) . . ?
O2 C1 Rh 175.1(3) . . ?
O1 C2 C3 122.9(3) . . ?
O1 C2 C4 114.4(2) . . ?
C3 C2 C4 122.5(3) . . ?
C2 C3 P2 114.7(2) . . ?
C5 C4 C9 117.3(3) . . ?
C5 C4 C2 120.3(3) . . ?
C9 C4 C2 122.1(3) . . ?
C4 C5 C6 121.8(4) . . ?
C7 C6 C5 119.9(4) . . ?
C6 C7 C8 119.8(4) . . ?
C9 C8 C7 120.4(4) . . ?
C8 C9 C4 120.8(4) . . ?
C15 C10 C11 117.9(3) . . ?
C15 C10 P2 120.8(3) . . ?
C11 C10 P2 121.1(2) . . ?
C12 C11 C10 121.2(4) . . ?
C13 C12 C11 120.1(4) . . ?
C12 C13 C14 120.0(4) . . ?
C13 C14 C15 120.5(4) . . ?
C10 C15 C14 120.3(4) . . ?
C17 C16 C21 119.5(3) . . ?
C17 C16 P2 120.8(3) . . ?
C21 C16 P2 119.6(3) . . ?
C16 C17 C18 119.8(4) . . ?
C19 C18 C17 120.5(5) . . ?
C18 C19 C20 120.5(4) . . ?
C19 C20 C21 119.3(5) . . ?
C16 C21 C20 120.3(5) . . ?
C27 C22 C23 118.6(3) . . ?
C27 C22 P1 122.6(2) . . ?
C23 C22 P1 118.8(2) . . ?
C22 C23 C24 120.6(3) . . ?
C25 C24 C23 120.3(4) . . ?
C24 C25 C26 119.8(3) . . ?
C25 C26 C27 120.8(4) . . ?
C22 C27 C26 120.0(3) . . ?
C33 C28 C29 118.7(3) . . ?
C33 C28 P1 117.8(2) . . ?
C29 C28 P1 123.5(2) . . ?
C30 C29 C28 119.8(3) . . ?
C31 C30 C29 120.5(3) . . ?
C30 C31 C32 119.9(3) . . ?
C33 C32 C31 120.0(3) . . ?
C32 C33 C28 121.1(3) . . ?
C39 C34 C35 118.5(3) . . ?
C39 C34 P1 122.2(2) . . ?
C35 C34 P1 119.3(2) . . ?
C34 C35 C36 120.8(3) . . ?
C37 C36 C35 119.9(3) . . ?
C36 C37 C38 120.0(3) . . ?
C37 C38 C39 120.5(3) . . ?
C34 C39 C38 120.1(3) . . ?
O3 C200 C300 150.6(50) . . ?
O3 C200 O3 44.3(34) . 3_654 ?
C300 C200 O3 163.0(34) . 3_654 ?
C200 O3 O3 96.9(32) . 3_654 ?
C200 O3 C200 135.7(34) . 3_654 ?
O3 O3 C200 38.8(34) 3_654 3_654 ?
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
Rh C1 1.803(3) . ?
Rh O1 2.059(2) . ?
Rh P2 2.2793(9) . ?
Rh P1 2.3588(8) . ?
P1 C28 1.824(3) . ?
P1 C22 1.826(3) . ?
P1 C34 1.834(3) . ?
P2 C3 1.761(3) . ?
P2 C10 1.823(3) . ?
P2 C16 1.825(3) . ?
O1 C2 1.320(4) . ?
O2 C1 1.151(4) . ?
C2 C3 1.363(4) . ?
C2 C4 1.491(4) . ?
C4 C5 1.377(5) . ?
C4 C9 1.385(5) . ?
C5 C6 1.385(5) . ?
C6 C7 1.348(6) . ?
C7 C8 1.378(6) . ?
C8 C9 1.375(6) . ?
C10 C15 1.384(4) . ?
C10 C11 1.390(5) . ?
C11 C12 1.386(5) . ?
C12 C13 1.360(6) . ?
C13 C14 1.370(6) . ?
C14 C15 1.393(5) . ?
C16 C17 1.367(5) . ?
C16 C21 1.385(5) . ?
C17 C18 1.396(5) . ?
C18 C19 1.354(8) . ?
C19 C20 1.374(8) . ?
C20 C21 1.389(6) . ?
C22 C27 1.381(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.388(5) . ?
C24 C25 1.362(6) . ?
C25 C26 1.363(6) . ?
C26 C27 1.395(5) . ?
C28 C33 1.384(4) . ?
C28 C29 1.398(4) . ?
C29 C30 1.383(5) . ?
C30 C31 1.377(5) . ?
C31 C32 1.376(6) . ?
C32 C33 1.375(5) . ?
C34 C39 1.381(4) . ?
C34 C35 1.384(4) . ?
C35 C36 1.389(5) . ?
C36 C37 1.362(5) . ?
C37 C38 1.369(6) . ?
C38 C39 1.389(5) . ?
C200 O3 0.96(5) . ?
C200 C300 1.19(3) . ?
C200 O3 1.52(5) 3_654 ?
O3 O3 1.07(8) 3_654 ?
O3 C200 1.52(5) 3_654 ?
