#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:49:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179709 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/12/7001230.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_7001230
loop_
_publ_author_name
'Vicente, José'
'Gil-Rubio, Juan'
'Guerrero-Leal, Juan'
'Bautista, Delia'
_publ_section_title
;
 Synthesis of rhodium(i) and rhodium(iii) perfluoroalkyl complexes from
 [Rh(μ-OH)(COD)]2
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3854
_journal_page_last               3866
_journal_paper_doi               10.1039/b822738a
_journal_year                    2009
_chemical_formula_sum            'C29 H34 F7 I N P2 Rh'
_chemical_formula_weight         821.32
_chemical_name_systematic
;
?
;
_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                88.019(2)
_cell_angle_beta                 76.668(2)
_cell_angle_gamma                69.908(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4084(5)
_cell_length_b                   11.6334(5)
_cell_length_c                   13.1497(6)
_cell_measurement_reflns_used    6798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.48
_cell_volume                     1592.92(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω-scan
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18039
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_T_max  0.7881
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         7093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0234P)²+0.8200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0474
_reflns_number_gt                6838
_reflns_number_total             7093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822738a.txt
_cod_data_source_block           jgl2382s
_cod_database_code               7001230
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 0.679280(11) 0.111052(10) 0.260489(9) 0.01112(4) Uani 1 1 d . . .
I2 I 0.763303(10) 0.269480(9) 0.121106(8) 0.01588(4) Uani 1 1 d . . .
P3 P 0.60854(4) 0.25494(4) 0.40253(3) 0.01375(8) Uani 1 1 d . . .
P4 P 0.73898(4) -0.03656(4) 0.12138(3) 0.01617(9) Uani 1 1 d . . .
F1 F 0.96136(9) 0.01700(9) 0.21028(8) 0.0204(2) Uani 1 1 d . . .
F2 F 0.88351(9) 0.11956(9) 0.36028(8) 0.0199(2) Uani 1 1 d . . .
F3 F 0.86568(10) -0.16859(9) 0.31189(9) 0.0240(2) Uani 1 1 d . . .
F4 F 0.83083(10) -0.06291(10) 0.45705(8) 0.0249(2) Uani 1 1 d . . .
F5 F 1.05013(12) -0.23490(11) 0.42620(11) 0.0366(3) Uani 1 1 d . . .
F6 F 1.11122(12) -0.19634(12) 0.26593(11) 0.0414(3) Uani 1 1 d . . .
F7 F 1.08830(12) -0.06810(11) 0.38924(12) 0.0404(3) Uani 1 1 d . . .
C1 C 0.59122(16) 0.00694(15) 0.36598(13) 0.0175(3) Uani 1 1 d . . .
H1A H 0.4992 0.0530 0.3895 0.026 Uiso 1 1 calc R . .
H1B H 0.6301 -0.0097 0.4265 0.026 Uiso 1 1 calc R . .
H1C H 0.6036 -0.0707 0.3308 0.026 Uiso 1 1 calc R . .
C2 C 0.85965(16) 0.03851(15) 0.29797(13) 0.0163(3) Uani 1 1 d . . .
C3 C 0.89676(17) -0.08248(15) 0.35578(14) 0.0196(3) Uani 1 1 d . . .
C4 C 1.03940(18) -0.14518(17) 0.35894(17) 0.0281(4) Uani 1 1 d . . .
C5 C 0.51226(15) 0.18372(14) 0.22140(12) 0.0141(3) Uani 1 1 d . . .
N1 N 0.41417(13) 0.22660(13) 0.19983(11) 0.0165(3) Uani 1 1 d . . .
C11 C 0.29464(16) 0.28684(15) 0.17612(13) 0.0168(3) Uani 1 1 d . . .
C12 C 0.28355(17) 0.38564(16) 0.11056(14) 0.0193(3) Uani 1 1 d . . .
C13 C 0.16374(18) 0.44373(18) 0.08854(16) 0.0264(4) Uani 1 1 d . . .
H13 H 0.1518 0.5117 0.0450 0.032 Uiso 1 1 calc R . .
C14 C 0.06185(19) 0.4039(2) 0.12920(17) 0.0304(4) Uani 1 1 d . . .
H14 H -0.0185 0.4436 0.1120 0.036 Uiso 1 1 calc R . .
C15 C 0.07601(18) 0.30654(19) 0.19479(16) 0.0273(4) Uani 1 1 d . . .
H15 H 0.0050 0.2808 0.2224 0.033 Uiso 1 1 calc R . .
C16 C 0.19305(17) 0.24608(17) 0.22063(14) 0.0206(3) Uani 1 1 d . . .
C17 C 0.39467(18) 0.42777(18) 0.06744(15) 0.0247(4) Uani 1 1 d . . .
H17A H 0.3705 0.4927 0.0188 0.037 Uiso 1 1 calc R . .
H17B H 0.4680 0.3587 0.0304 0.037 Uiso 1 1 calc R . .
H17C H 0.4182 0.4595 0.1249 0.037 Uiso 1 1 calc R . .
C18 C 0.2089(2) 0.1435(2) 0.29491(17) 0.0297(4) Uani 1 1 d . . .
H18A H 0.1263 0.1319 0.3213 0.045 Uiso 1 1 calc R . .
H18B H 0.2389 0.1640 0.3536 0.045 Uiso 1 1 calc R . .
H18C H 0.2719 0.0678 0.2581 0.045 Uiso 1 1 calc R . .
C21 C 0.43785(16) 0.34219(15) 0.42345(13) 0.0167(3) Uani 1 1 d . . .
C22 C 0.39816(17) 0.43392(16) 0.35458(14) 0.0203(3) Uani 1 1 d . . .
H22 H 0.4604 0.4512 0.3007 0.024 Uiso 1 1 calc R . .
C23 C 0.26925(18) 0.49984(17) 0.36404(16) 0.0254(4) Uani 1 1 d . . .
H23 H 0.2435 0.5618 0.3167 0.030 Uiso 1 1 calc R . .
C24 C 0.17809(18) 0.47583(18) 0.44202(19) 0.0323(5) Uani 1 1 d . . .
H24 H 0.0896 0.5212 0.4485 0.039 Uiso 1 1 calc R . .
C25 C 0.21604(19) 0.38522(19) 0.51103(19) 0.0353(5) Uani 1 1 d . . .
H25 H 0.1533 0.3689 0.5650 0.042 Uiso 1 1 calc R . .
C26 C 0.34569(18) 0.31803(17) 0.50167(16) 0.0250(4) Uani 1 1 d . . .
H26 H 0.3710 0.2557 0.5489 0.030 Uiso 1 1 calc R . .
C27 C 0.67830(17) 0.37497(16) 0.39374(15) 0.0212(4) Uani 1 1 d . . .
H27A H 0.6641 0.4210 0.3312 0.032 Uiso 1 1 calc R . .
H27B H 0.7707 0.3381 0.3891 0.032 Uiso 1 1 calc R . .
H27C H 0.6378 0.4305 0.4561 0.032 Uiso 1 1 calc R . .
C28 C 0.62454(18) 0.19904(17) 0.53136(13) 0.0211(4) Uani 1 1 d . . .
H28A H 0.5848 0.2677 0.5835 0.032 Uiso 1 1 calc R . .
H28B H 0.7157 0.1608 0.5311 0.032 Uiso 1 1 calc R . .
H28C H 0.5817 0.1385 0.5488 0.032 Uiso 1 1 calc R . .
C31 C 0.67044(18) -0.15769(16) 0.14889(13) 0.0195(3) Uani 1 1 d . . .
C32 C 0.53941(19) -0.12930(18) 0.15759(15) 0.0255(4) Uani 1 1 d . . .
H32 H 0.4878 -0.0477 0.1485 0.031 Uiso 1 1 calc R . .
C33 C 0.4833(2) -0.2186(2) 0.17938(16) 0.0339(5) Uani 1 1 d . . .
H33 H 0.3940 -0.1986 0.1844 0.041 Uiso 1 1 calc R . .
C34 C 0.5585(2) -0.3375(2) 0.19384(16) 0.0360(5) Uani 1 1 d . . .
H34 H 0.5206 -0.3992 0.2083 0.043 Uiso 1 1 calc R . .
C35 C 0.6873(2) -0.36639(18) 0.18728(17) 0.0344(5) Uani 1 1 d . . .
H35 H 0.7380 -0.4477 0.1981 0.041 Uiso 1 1 calc R . .
C36 C 0.7438(2) -0.27718(17) 0.16482(15) 0.0272(4) Uani 1 1 d . . .
H36 H 0.8331 -0.2978 0.1603 0.033 Uiso 1 1 calc R . .
C37 C 0.90661(18) -0.11885(18) 0.06157(16) 0.0273(4) Uani 1 1 d . . .
H37A H 0.9491 -0.1652 0.1145 0.041 Uiso 1 1 calc R . .
H37B H 0.9485 -0.0603 0.0324 0.041 Uiso 1 1 calc R . .
H37C H 0.9127 -0.1754 0.0055 0.041 Uiso 1 1 calc R . .
C38 C 0.6823(2) 0.02663(18) 0.00562(14) 0.0268(4) Uani 1 1 d . . .
H38A H 0.7218 0.0873 -0.0224 0.040 Uiso 1 1 calc R . .
H38B H 0.5887 0.0660 0.0246 0.040 Uiso 1 1 calc R . .
H38C H 0.7059 -0.0395 -0.0475 0.040 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'
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'
I I -0.4742 1.8119 '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
C5 Rh1 C2 177.70(6) . . ?
C5 Rh1 C1 86.58(6) . . ?
C2 Rh1 C1 95.71(6) . . ?
C5 Rh1 P3 90.46(5) . . ?
C2 Rh1 P3 89.62(5) . . ?
C1 Rh1 P3 84.89(5) . . ?
C5 Rh1 P4 87.40(5) . . ?
C2 Rh1 P4 92.63(5) . . ?
C1 Rh1 P4 92.25(5) . . ?
P3 Rh1 P4 176.529(15) . . ?
C5 Rh1 I2 86.37(5) . . ?
C2 Rh1 I2 91.33(4) . . ?
C1 Rh1 I2 172.52(5) . . ?
P3 Rh1 I2 92.650(11) . . ?
P4 Rh1 I2 89.943(12) . . ?
C27 P3 C28 101.48(9) . . ?
C27 P3 C21 102.38(8) . . ?
C28 P3 C21 103.03(8) . . ?
C27 P3 Rh1 117.84(6) . . ?
C28 P3 Rh1 118.35(6) . . ?
C21 P3 Rh1 111.58(6) . . ?
C37 P4 C31 103.50(9) . . ?
C37 P4 C38 99.95(10) . . ?
C31 P4 C38 101.48(9) . . ?
C37 P4 Rh1 120.98(7) . . ?
C31 P4 Rh1 114.84(6) . . ?
C38 P4 Rh1 113.39(6) . . ?
F1 C2 F2 102.12(12) . . ?
F1 C2 C3 103.12(13) . . ?
F2 C2 C3 102.51(13) . . ?
F1 C2 Rh1 112.67(11) . . ?
F2 C2 Rh1 113.29(10) . . ?
C3 C2 Rh1 120.94(11) . . ?
F4 C3 F3 107.70(14) . . ?
F4 C3 C4 105.50(14) . . ?
F3 C3 C4 105.13(14) . . ?
F4 C3 C2 109.76(14) . . ?
F3 C3 C2 110.31(14) . . ?
C4 C3 C2 117.89(15) . . ?
F7 C4 F6 108.34(17) . . ?
F7 C4 F5 107.80(16) . . ?
F6 C4 F5 107.01(15) . . ?
F7 C4 C3 112.37(15) . . ?
F6 C4 C3 111.56(16) . . ?
F5 C4 C3 109.56(16) . . ?
N1 C5 Rh1 179.19(15) . . ?
C5 N1 C11 175.92(16) . . ?
C16 C11 C12 123.77(16) . . ?
C16 C11 N1 118.17(15) . . ?
C12 C11 N1 118.04(15) . . ?
C13 C12 C11 116.75(16) . . ?
C13 C12 C17 121.69(16) . . ?
C11 C12 C17 121.55(16) . . ?
C14 C13 C12 121.02(18) . . ?
C13 C14 C15 120.63(17) . . ?
C14 C15 C16 120.85(18) . . ?
C15 C16 C11 116.95(17) . . ?
C15 C16 C18 121.61(17) . . ?
C11 C16 C18 121.42(16) . . ?
C26 C21 C22 118.91(16) . . ?
C26 C21 P3 122.88(13) . . ?
C22 C21 P3 118.15(13) . . ?
C23 C22 C21 120.71(17) . . ?
C24 C23 C22 120.18(18) . . ?
C23 C24 C25 119.75(18) . . ?
C24 C25 C26 120.39(19) . . ?
C21 C26 C25 120.05(17) . . ?
C36 C31 C32 118.69(17) . . ?
C36 C31 P4 122.22(15) . . ?
C32 C31 P4 119.06(14) . . ?
C33 C32 C31 120.86(19) . . ?
C32 C33 C34 119.5(2) . . ?
C35 C34 C33 120.30(19) . . ?
C34 C35 C36 120.3(2) . . ?
C35 C36 C31 120.4(2) . . ?
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 C5 1.9810(16) . ?
Rh1 C2 2.1061(16) . ?
Rh1 C1 2.1160(16) . ?
Rh1 P3 2.3526(4) . ?
Rh1 P4 2.3660(4) . ?
Rh1 I2 2.80090(18) . ?
P3 C27 1.8184(18) . ?
P3 C28 1.8196(17) . ?
P3 C21 1.8200(17) . ?
P4 C37 1.8146(19) . ?
P4 C31 1.8219(17) . ?
P4 C38 1.8237(19) . ?
F1 C2 1.3936(19) . ?
F2 C2 1.4025(19) . ?
F3 C3 1.357(2) . ?
F4 C3 1.354(2) . ?
F5 C4 1.336(2) . ?
F6 C4 1.332(2) . ?
F7 C4 1.321(2) . ?
C2 C3 1.550(2) . ?
C3 C4 1.548(2) . ?
C5 N1 1.155(2) . ?
N1 C11 1.404(2) . ?
C11 C16 1.399(2) . ?
C11 C12 1.401(2) . ?
C12 C13 1.394(2) . ?
C12 C17 1.498(2) . ?
C13 C14 1.385(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.393(3) . ?
C16 C18 1.504(3) . ?
C21 C26 1.388(2) . ?
C21 C22 1.398(2) . ?
C22 C23 1.383(3) . ?
C23 C24 1.378(3) . ?
C24 C25 1.387(3) . ?
C25 C26 1.394(3) . ?
C31 C36 1.392(3) . ?
C31 C32 1.393(3) . ?
C32 C33 1.387(3) . ?
C33 C34 1.388(3) . ?
C34 C35 1.373(3) . ?
C35 C36 1.390(3) . ?
