#------------------------------------------------------------------------------
#$Date: 2018-09-04 17:33:05 +0200 (mar 04 de sep de 2018) $
#$Revision: 210422 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/27/7102760.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_7102760
loop_
_publ_author_name
'Geier, Stephen J.'
'Stephan, Douglas W.'
_publ_section_title
;
 Rh-catalyzed P--P bond activation
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              99
_journal_page_last               101
_journal_paper_doi               10.1039/b712972f
_journal_year                    2008
_chemical_formula_sum            'C37 H61 N2 P2 Rh'
_chemical_formula_weight         698.73
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.412(4)
_cell_angle_beta                 93.045(4)
_cell_angle_gamma                114.125(4)
_cell_formula_units_Z            2
_cell_length_a                   10.566(3)
_cell_length_b                   11.676(4)
_cell_length_c                   17.636(6)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     1914.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.158795
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1137P)²+0.1449P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                6106
_reflns_number_total             6726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712972f.txt
_cod_data_source_block           RhNacNac(Et2PPEt2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7102760
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.06574(2) 0.277892(18) -0.271033(12) 0.06049(12) Uani 1 1 d . . .
P1 P -0.02460(8) 0.41981(8) -0.22896(5) 0.0715(2) Uani 1 1 d . . .
P2 P -0.15441(9) 0.21786(9) -0.24861(6) 0.0793(2) Uani 1 1 d . . .
N1 N 0.2670(2) 0.3810(2) -0.29148(13) 0.0577(5) Uani 1 1 d . . .
N2 N 0.0972(2) 0.1115(2) -0.28887(14) 0.0616(5) Uani 1 1 d . . .
C1 C 0.3165(3) 0.5195(3) -0.27876(16) 0.0620(6) Uani 1 1 d . . .
C2 C 0.3702(3) 0.6000(3) -0.20141(18) 0.0697(7) Uani 1 1 d . . .
C3 C 0.4165(4) 0.7335(3) -0.1917(2) 0.0857(9) Uani 1 1 d . . .
H3A H 0.4521 0.7888 -0.1414 0.103 Uiso 1 1 calc R . .
C4 C 0.4114(4) 0.7858(3) -0.2532(3) 0.0918(10) Uani 1 1 d . . .
H4A H 0.4440 0.8753 -0.2446 0.110 Uiso 1 1 calc R . .
C5 C 0.3583(4) 0.7064(3) -0.3277(2) 0.0842(9) Uani 1 1 d . . .
H5A H 0.3547 0.7429 -0.3693 0.101 Uiso 1 1 calc R . .
C6 C 0.3092(3) 0.5713(3) -0.34262(18) 0.0690(7) Uani 1 1 d . . .
C7 C 0.3755(4) 0.5420(4) -0.13307(19) 0.0849(9) Uani 1 1 d . . .
H7A H 0.2864 0.4645 -0.1409 0.102 Uiso 1 1 calc R . .
C8 C 0.3868(5) 0.6330(5) -0.0524(2) 0.1199(16) Uani 1 1 d . . .
H8A H 0.3916 0.5917 -0.0115 0.180 Uiso 1 1 calc R . .
H8B H 0.3058 0.6508 -0.0518 0.180 Uiso 1 1 calc R . .
H8C H 0.4700 0.7130 -0.0439 0.180 Uiso 1 1 calc R . .
C9 C 0.4919(5) 0.4970(5) -0.1301(3) 0.1049(12) Uani 1 1 d . . .
H9A H 0.4832 0.4386 -0.1797 0.157 Uiso 1 1 calc R . .
H9B H 0.4842 0.4531 -0.0892 0.157 Uiso 1 1 calc R . .
H9C H 0.5816 0.5709 -0.1196 0.157 Uiso 1 1 calc R . .
C10 C 0.2459(4) 0.4842(3) -0.42479(19) 0.0795(8) Uani 1 1 d . . .
H10A H 0.2593 0.4051 -0.4279 0.095 Uiso 1 1 calc R . .
C11 C 0.0878(5) 0.4437(5) -0.4382(3) 0.1158(15) Uani 1 1 d . . .
H11A H 0.0467 0.4058 -0.3971 0.174 Uiso 1 1 calc R . .
H11B H 0.0465 0.3812 -0.4881 0.174 Uiso 1 1 calc R . .
H11C H 0.0710 0.5186 -0.4376 0.174 Uiso 1 1 calc R . .
C12 C 0.3162(8) 0.5441(5) -0.4889(3) 0.150(2) Uani 1 1 d . . .
H12A H 0.2732 0.4836 -0.5393 0.225 Uiso 1 1 calc R . .
H12B H 0.4143 0.5642 -0.4804 0.225 Uiso 1 1 calc R . .
H12C H 0.3055 0.6223 -0.4873 0.225 Uiso 1 1 calc R . .
C13 C 0.4928(3) 0.4160(3) -0.3377(2) 0.0799(8) Uani 1 1 d . . .
H13A H 0.4794 0.4292 -0.3889 0.120 Uiso 1 1 calc R . .
H13B H 0.5545 0.3743 -0.3373 0.120 Uiso 1 1 calc R . .
H13C H 0.5335 0.4984 -0.2992 0.120 Uiso 1 1 calc R . .
C14 C 0.3518(3) 0.3305(3) -0.31841(17) 0.0640(6) Uani 1 1 d . . .
C15 C 0.3237(3) 0.1998(3) -0.32866(18) 0.0675(7) Uani 1 1 d . . .
H15A H 0.3901 0.1757 -0.3506 0.081 Uiso 1 1 calc R . .
C16 C 0.2107(3) 0.1006(3) -0.31069(17) 0.0661(6) Uani 1 1 d . . .
C17 C 0.2270(4) -0.0244(3) -0.3145(2) 0.0870(9) Uani 1 1 d . . .
H17A H 0.2952 -0.0103 -0.2711 0.131 Uiso 1 1 calc R . .
H17B H 0.2578 -0.0494 -0.3630 0.131 Uiso 1 1 calc R . .
H17C H 0.1384 -0.0923 -0.3117 0.131 Uiso 1 1 calc R . .
C18 C -0.0035(3) 0.0077(3) -0.26282(18) 0.0662(6) Uani 1 1 d . . .
C19 C -0.1287(3) -0.0815(3) -0.3134(2) 0.0736(7) Uani 1 1 d . . .
C20 C -0.2274(4) -0.1741(3) -0.2833(3) 0.0913(10) Uani 1 1 d . . .
H20A H -0.3109 -0.2341 -0.3157 0.110 Uiso 1 1 calc R . .
C21 C -0.2054(4) -0.1799(4) -0.2066(3) 0.0946(11) Uani 1 1 d . . .
H21A H -0.2745 -0.2418 -0.1877 0.114 Uiso 1 1 calc R . .
C22 C -0.0828(4) -0.0953(4) -0.1590(2) 0.0888(10) Uani 1 1 d . . .
H22A H -0.0684 -0.1012 -0.1077 0.107 Uiso 1 1 calc R . .
C23 C 0.0223(3) 0.0006(3) -0.18504(19) 0.0741(7) Uani 1 1 d . . .
C24 C -0.1530(4) -0.0760(3) -0.3983(2) 0.0862(9) Uani 1 1 d . . .
H24A H -0.1215 0.0155 -0.3980 0.103 Uiso 1 1 calc R . .
C25 C -0.3091(5) -0.1490(5) -0.4365(3) 0.1189(15) Uani 1 1 d . . .
H25A H -0.3180 -0.1423 -0.4896 0.178 Uiso 1 1 calc R . .
H25B H -0.3628 -0.1112 -0.4072 0.178 Uiso 1 1 calc R . .
H25C H -0.3436 -0.2389 -0.4364 0.178 Uiso 1 1 calc R . .
C26 C -0.0697(5) -0.1299(5) -0.4511(3) 0.1165(14) Uani 1 1 d . . .
H26A H -0.0912 -0.1267 -0.5040 0.175 Uiso 1 1 calc R . .
H26B H -0.0945 -0.2183 -0.4501 0.175 Uiso 1 1 calc R . .
H26C H 0.0289 -0.0786 -0.4326 0.175 Uiso 1 1 calc R . .
C27 C 0.1578(4) 0.0941(4) -0.1302(2) 0.0885(9) Uani 1 1 d . . .
H27A H 0.2250 0.1387 -0.1622 0.106 Uiso 1 1 calc R . .
C28 C 0.1357(6) 0.1977(5) -0.0702(3) 0.1149(14) Uani 1 1 d . . .
H28A H 0.0949 0.2406 -0.0973 0.172 Uiso 1 1 calc R . .
H28B H 0.2244 0.2602 -0.0395 0.172 Uiso 1 1 calc R . .
H28C H 0.0738 0.1572 -0.0362 0.172 Uiso 1 1 calc R . .
C29 C 0.2219(6) 0.0222(6) -0.0893(3) 0.1275(16) Uani 1 1 d . . .
H29A H 0.2334 -0.0429 -0.1281 0.191 Uiso 1 1 calc R . .
H29B H 0.1607 -0.0185 -0.0551 0.191 Uiso 1 1 calc R . .
H29C H 0.3117 0.0830 -0.0591 0.191 Uiso 1 1 calc R . .
C30 C -0.0970(4) 0.5068(4) -0.2802(3) 0.0884(10) Uani 1 1 d . . .
H30A H -0.1260 0.4608 -0.3355 0.106 Uiso 1 1 calc R . .
H30B H -0.1795 0.5070 -0.2588 0.106 Uiso 1 1 calc R . .
C31 C 0.0091(5) 0.6472(4) -0.2724(3) 0.1075(13) Uani 1 1 d . . .
H31A H -0.0339 0.6890 -0.2990 0.161 Uiso 1 1 calc R . .
H31B H 0.0893 0.6474 -0.2956 0.161 Uiso 1 1 calc R . .
H31C H 0.0382 0.6931 -0.2178 0.161 Uiso 1 1 calc R . .
C32 C 0.0121(5) 0.5120(5) -0.1268(3) 0.1023(12) Uani 1 1 d . . .
H32A H 0.0322 0.4619 -0.0946 0.123 Uiso 1 1 calc R . .
H32B H 0.0971 0.5913 -0.1201 0.123 Uiso 1 1 calc R . .
C33 C -0.1004(6) 0.5492(6) -0.0941(3) 0.1336(18) Uani 1 1 d . . .
H33A H -0.0663 0.6001 -0.0406 0.200 Uiso 1 1 calc R . .
H33B H -0.1834 0.4719 -0.0961 0.200 Uiso 1 1 calc R . .
H33C H -0.1221 0.5991 -0.1250 0.200 Uiso 1 1 calc R . .
C34 C -0.2240(5) 0.1628(5) -0.1642(3) 0.1123(14) Uani 1 1 d . . .
H34A H -0.2403 0.0727 -0.1730 0.135 Uiso 1 1 calc R . .
H34B H -0.1514 0.2121 -0.1186 0.135 Uiso 1 1 calc R . .
C35 C -0.3591(6) 0.1719(6) -0.1430(4) 0.161(3) Uani 1 1 d . . .
H35A H -0.3856 0.1358 -0.0992 0.242 Uiso 1 1 calc R . .
H35B H -0.4329 0.1243 -0.1873 0.242 Uiso 1 1 calc R . .
H35C H -0.3433 0.2613 -0.1294 0.242 Uiso 1 1 calc R . .
C36 C -0.3134(4) 0.1533(4) -0.3215(3) 0.1130(15) Uani 1 1 d . . .
H36A H -0.3636 0.0608 -0.3267 0.136 Uiso 1 1 calc R . .
H36B H -0.3734 0.1934 -0.3015 0.136 Uiso 1 1 calc R . .
C37 C -0.2899(6) 0.1736(5) -0.4030(4) 0.1312(19) Uani 1 1 d . . .
H37A H -0.3788 0.1364 -0.4368 0.197 Uiso 1 1 calc R . .
H37B H -0.2329 0.1323 -0.4243 0.197 Uiso 1 1 calc R . .
H37C H -0.2433 0.2650 -0.3993 0.197 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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
N2 Rh1 N1 90.30(9) . . ?
N2 Rh1 P2 105.36(7) . . ?
N1 Rh1 P2 164.24(7) . . ?
N2 Rh1 P1 160.10(7) . . ?
N1 Rh1 P1 108.03(7) . . ?
P2 Rh1 P1 56.77(4) . . ?
C32 P1 C30 103.0(2) . . ?
C32 P1 P2 114.21(18) . . ?
C30 P1 P2 115.15(13) . . ?
C32 P1 Rh1 122.09(15) . . ?
C30 P1 Rh1 132.61(15) . . ?
P2 P1 Rh1 61.06(4) . . ?
C34 P2 C36 102.4(3) . . ?
C34 P2 P1 116.75(18) . . ?
C36 P2 P1 115.11(17) . . ?
C34 P2 Rh1 126.51(18) . . ?
C36 P2 Rh1 127.41(19) . . ?
P1 P2 Rh1 62.17(3) . . ?
C14 N1 C1 117.0(2) . . ?
C14 N1 Rh1 125.62(19) . . ?
C1 N1 Rh1 117.34(16) . . ?
C16 N2 C18 118.3(2) . . ?
C16 N2 Rh1 125.64(19) . . ?
C18 N2 Rh1 115.24(17) . . ?
C6 C1 C2 121.4(3) . . ?
C6 C1 N1 119.7(2) . . ?
C2 C1 N1 118.8(2) . . ?
C3 C2 C1 116.9(3) . . ?
C3 C2 C7 122.4(3) . . ?
C1 C2 C7 120.6(3) . . ?
C4 C3 C2 122.5(3) . . ?
C3 C4 C5 119.9(3) . . ?
C4 C5 C6 121.4(3) . . ?
C1 C6 C5 117.9(3) . . ?
C1 C6 C10 121.2(3) . . ?
C5 C6 C10 120.9(3) . . ?
C2 C7 C9 113.1(3) . . ?
C2 C7 C8 113.4(3) . . ?
C9 C7 C8 109.6(3) . . ?
C6 C10 C12 113.4(3) . . ?
C6 C10 C11 109.7(3) . . ?
C12 C10 C11 111.5(4) . . ?
N1 C14 C15 124.0(3) . . ?
N1 C14 C13 120.4(3) . . ?
C15 C14 C13 115.5(3) . . ?
C16 C15 C14 129.3(3) . . ?
N2 C16 C15 124.1(3) . . ?
N2 C16 C17 120.5(3) . . ?
C15 C16 C17 115.3(3) . . ?
C19 C18 C23 121.2(3) . . ?
C19 C18 N2 119.9(3) . . ?
C23 C18 N2 118.9(3) . . ?
C20 C19 C18 117.5(3) . . ?
C20 C19 C24 121.8(3) . . ?
C18 C19 C24 120.6(3) . . ?
C21 C20 C19 122.0(4) . . ?
C22 C21 C20 119.9(3) . . ?
C21 C22 C23 121.6(4) . . ?
C22 C23 C18 117.8(3) . . ?
C22 C23 C27 120.3(3) . . ?
C18 C23 C27 121.9(3) . . ?
C19 C24 C26 113.0(3) . . ?
C19 C24 C25 113.1(3) . . ?
C26 C24 C25 107.7(3) . . ?
C23 C27 C28 111.2(3) . . ?
C23 C27 C29 111.6(3) . . ?
C28 C27 C29 111.2(4) . . ?
C31 C30 P1 112.5(3) . . ?
C33 C32 P1 118.0(4) . . ?
C35 C34 P2 118.7(4) . . ?
C37 C36 P2 115.7(3) . . ?
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
Rh1 N2 2.064(2) . ?
Rh1 N1 2.068(2) . ?
Rh1 P2 2.2231(11) . ?
Rh1 P1 2.2465(10) . ?
P1 C32 1.819(4) . ?
P1 C30 1.840(4) . ?
P1 P2 2.1250(14) . ?
P2 C34 1.819(5) . ?
P2 C36 1.834(4) . ?
N1 C14 1.317(4) . ?
N1 C1 1.441(3) . ?
N2 C16 1.325(4) . ?
N2 C18 1.431(4) . ?
C1 C6 1.401(4) . ?
C1 C2 1.413(4) . ?
C2 C3 1.397(5) . ?
C2 C7 1.513(5) . ?
C3 C4 1.363(6) . ?
C4 C5 1.369(6) . ?
C5 C6 1.402(4) . ?
C6 C10 1.513(5) . ?
C7 C9 1.524(6) . ?
C7 C8 1.548(5) . ?
C10 C12 1.524(5) . ?
C10 C11 1.527(6) . ?
C13 C14 1.522(4) . ?
C14 C15 1.398(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.527(4) . ?
C18 C19 1.407(4) . ?
C18 C23 1.411(4) . ?
C19 C20 1.387(5) . ?
C19 C24 1.524(5) . ?
C20 C21 1.381(6) . ?
C21 C22 1.357(6) . ?
C22 C23 1.399(5) . ?
C23 C27 1.515(5) . ?
C24 C26 1.525(6) . ?
C24 C25 1.545(5) . ?
C27 C28 1.532(6) . ?
C27 C29 1.536(6) . ?
C30 C31 1.532(5) . ?
C32 C33 1.523(6) . ?
C34 C35 1.533(7) . ?
C36 C37 1.523(8) . ?
