#------------------------------------------------------------------------------
#$Date: 2017-03-04 16:05:09 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193520 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/54/4125415.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_4125415
loop_
_publ_author_name
'Piou, Tiffany'
'Romanov-Michailidis, Fedor'
'Romanova-Michaelides, Maria'
'Jackson, Kelvin E.'
'Semakul, Natthawat'
'Taggart, Trevor D.'
'Newell, Brian S.'
'Rithner, Christopher D.'
'Paton, Robert S.'
'Rovis, Tomislav'
_publ_section_title
;
 Correlating Reactivity and Selectivity to Cyclopentadienyl Ligand
 Properties in Rh(III)-Catalyzed C-H Activation Reactions: An Experimental
 and Computational Study.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1296
_journal_page_last               1310
_journal_paper_doi               10.1021/jacs.6b11670
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C30 H46 Cl4 Rh2'
_chemical_formula_sum            'C30 H46 Cl4 Rh2'
_chemical_formula_weight         754.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.257(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6900(6)
_cell_length_b                   11.9817(9)
_cell_length_c                   16.7847(12)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.89
_cell_measurement_theta_min      2.69
_cell_volume                     1521.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58401
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.463
_diffrn_reflns_theta_min         2.100
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         6415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0375
_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)+(0.0334P)²+1.9782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4935
_reflns_number_total             6415
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Rh3.cif
_cod_data_source_block           rovis192
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125410--4125429.cif.
;
_cod_database_code               4125415
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.654
_shelx_estimated_absorpt_t_max   0.856
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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
Rh1 Rh 0.44257(2) 0.09518(2) 0.41454(2) 0.01401(5) Uani 1 1 d . . . . .
Cl1 Cl 0.63745(8) -0.00348(5) 0.34340(4) 0.02302(12) Uani 1 1 d . . . . .
Cl2 Cl 0.33755(7) -0.08258(4) 0.45997(3) 0.01723(10) Uani 1 1 d . . . . .
C1 C 0.2244(4) 0.1571(2) 0.32960(18) 0.0354(8) Uani 1 1 d . . . . .
C2 C 0.1919(3) 0.1771(2) 0.41055(19) 0.0271(6) Uani 1 1 d . . . . .
C3 C 0.3282(3) 0.24586(18) 0.45181(14) 0.0171(4) Uani 1 1 d . . . . .
C4 C 0.4487(3) 0.27088(18) 0.39727(14) 0.0173(4) Uani 1 1 d . . . . .
C5 C 0.3818(4) 0.2182(2) 0.32158(15) 0.0298(6) Uani 1 1 d . . . . .
C6 C 0.1505(8) 0.1090(5) 0.2425(4) 0.0232(15) Uani 0.435(8) 1 d . . P A 1
H6A H 0.2356 0.1174 0.2043 0.028 Uiso 0.435(8) 1 calc R U P A 1
C7 C -0.024(4) 0.176(3) 0.216(2) 0.032(3) Uani 0.435(8) 1 d . . P A 1
H7A H -0.0736 0.1938 0.2645 0.038 Uiso 0.435(8) 1 calc R U P A 1
H7B H 0.0067 0.2476 0.1921 0.038 Uiso 0.435(8) 1 calc R U P A 1
C8 C -0.1708(12) 0.1188(7) 0.1533(6) 0.0270(18) Uani 0.435(8) 1 d . . P A 1
H8A H -0.2274 0.1744 0.1133 0.032 Uiso 0.435(8) 1 calc R U P A 1
H8B H -0.2626 0.0878 0.1816 0.032 Uiso 0.435(8) 1 calc R U P A 1
C9 C -0.0874(9) 0.0221(5) 0.1085(3) 0.0161(12) Uani 0.435(8) 1 d . . P A 1
H9A H -0.1774 -0.0145 0.0673 0.019 Uiso 0.435(8) 1 calc R U P A 1
H9B H 0.0097 0.0502 0.0824 0.019 Uiso 0.435(8) 1 calc R U P A 1
C10 C -0.019(5) -0.057(3) 0.178(2) 0.024(2) Uani 0.435(8) 1 d . . P A 1
H10A H -0.1216 -0.0929 0.1952 0.029 Uiso 0.435(8) 1 calc R U P A 1
H10B H 0.0511 -0.1158 0.1573 0.029 Uiso 0.435(8) 1 calc R U P A 1
C11 C 0.0881(16) -0.0071(9) 0.2477(7) 0.039(3) Uani 0.435(8) 1 d . . P A 1
H11A H 0.1936 -0.0550 0.2634 0.047 Uiso 0.435(8) 1 calc R U P A 1
H11B H 0.0203 -0.0103 0.2926 0.047 Uiso 0.435(8) 1 calc R U P A 1
C6A C 0.0750(5) 0.0939(3) 0.2742(2) 0.0141(9) Uani 0.565(8) 1 d . . P A 2
H6C H -0.0195 0.0705 0.3047 0.017 Uiso 0.565(8) 1 calc R U P A 2
C7A C 0.001(3) 0.188(2) 0.2046(15) 0.032(3) Uani 0.565(8) 1 d . . P A 2
H7C H -0.0668 0.2446 0.2291 0.038 Uiso 0.565(8) 1 calc R U P A 2
H7D H 0.1031 0.2254 0.1881 0.038 Uiso 0.565(8) 1 calc R U P A 2
C8A C -0.1133(14) 0.1427(7) 0.1316(6) 0.052(3) Uani 0.565(8) 1 d . . P A 2
H8C H -0.2236 0.1871 0.1218 0.062 Uiso 0.565(8) 1 calc R U P A 2
H8D H -0.0528 0.1556 0.0850 0.062 Uiso 0.565(8) 1 calc R U P A 2
C9A C -0.1606(12) 0.0282(6) 0.1314(5) 0.048(2) Uani 0.565(8) 1 d . . P A 2
H9C H -0.2091 0.0059 0.0751 0.058 Uiso 0.565(8) 1 calc R U P A 2
H9D H -0.2564 0.0197 0.1633 0.058 Uiso 0.565(8) 1 calc R U P A 2
C10A C -0.006(4) -0.056(3) 0.1666(15) 0.024(2) Uani 0.565(8) 1 d . . P A 2
H10C H -0.0580 -0.1206 0.1903 0.029 Uiso 0.565(8) 1 calc R U P A 2
H10D H 0.0481 -0.0835 0.1211 0.029 Uiso 0.565(8) 1 calc R U P A 2
C11A C 0.1450(9) -0.0056(7) 0.2329(6) 0.0232(15) Uani 0.565(8) 1 d . . P A 2
H11C H 0.1883 -0.0636 0.2736 0.028 Uiso 0.565(8) 1 calc R U P A 2
H11D H 0.2452 0.0183 0.2072 0.028 Uiso 0.565(8) 1 calc R U P A 2
C12 C 0.0424(4) 0.1355(3) 0.4481(3) 0.0541(11) Uani 1 1 d . . . . .
H12A H 0.0864 0.1149 0.5046 0.081 Uiso 1 1 calc R U . . .
H12B H -0.0106 0.0700 0.4183 0.081 Uiso 1 1 calc R U . . .
H12C H -0.0469 0.1943 0.4461 0.081 Uiso 1 1 calc R U . . .
C13 C 0.3459(4) 0.2862(2) 0.53701(16) 0.0299(6) Uani 1 1 d . . . . .
H13A H 0.2716 0.3523 0.5386 0.045 Uiso 1 1 calc R U . . .
H13B H 0.4695 0.3055 0.5577 0.045 Uiso 1 1 calc R U . . .
H13C H 0.3081 0.2273 0.5707 0.045 Uiso 1 1 calc R U . . .
C14 C 0.6051(4) 0.3457(2) 0.4151(2) 0.0370(7) Uani 1 1 d . . . . .
H14A H 0.6916 0.3242 0.3815 0.055 Uiso 1 1 calc R U . . .
H14B H 0.6588 0.3392 0.4724 0.055 Uiso 1 1 calc R U . . .
H14C H 0.5680 0.4231 0.4031 0.055 Uiso 1 1 calc R U . . .
C15 C 0.4667(7) 0.2274(3) 0.24886(19) 0.0605(13) Uani 1 1 d . . . . .
H15A H 0.4255 0.2955 0.2189 0.091 Uiso 1 1 calc R U . . .
H15B H 0.4353 0.1623 0.2140 0.091 Uiso 1 1 calc R U . . .
H15C H 0.5954 0.2306 0.2658 0.091 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'
Cl Cl 0.1484 0.1585 '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_3
C4 Rh1 C1 66.31(9) .
C4 Rh1 C5 39.19(9) .
C1 Rh1 C5 39.46(13) .
C4 Rh1 C3 39.50(9) .
C1 Rh1 C3 65.68(9) .
C5 Rh1 C3 65.52(9) .
C4 Rh1 C2 65.55(9) .
C1 Rh1 C2 39.39(12) .
C5 Rh1 C2 65.48(12) .
C3 Rh1 C2 38.37(9) .
C4 Rh1 Cl1 112.99(6) .
C1 Rh1 Cl1 109.09(9) .
C5 Rh1 Cl1 92.94(8) .
C3 Rh1 Cl1 152.46(6) .
C2 Rh1 Cl1 147.97(8) .
C4 Rh1 Cl2 157.00(6) .
C1 Rh1 Cl2 104.32(9) .
C5 Rh1 Cl2 141.86(9) .
C3 Rh1 Cl2 117.74(6) .
C2 Rh1 Cl2 93.61(7) .
Cl1 Rh1 Cl2 89.79(2) .
C4 Rh1 Cl2 98.56(6) 3_656
C1 Rh1 Cl2 158.91(8) 3_656
C5 Rh1 Cl2 134.04(9) 3_656
C3 Rh1 Cl2 93.25(6) 3_656
C2 Rh1 Cl2 121.98(8) 3_656
Cl1 Rh1 Cl2 90.05(2) 3_656
Cl2 Rh1 Cl2 83.940(19) 3_656
Rh1 Cl2 Rh1 96.060(19) 3_656
C5 C1 C2 107.0(2) .
C5 C1 C6A 137.8(3) .
C2 C1 C6A 114.4(3) .
C5 C1 C6 105.6(4) .
C2 C1 C6 146.8(4) .
C5 C1 Rh1 70.44(14) .
C2 C1 Rh1 71.09(13) .
C6A C1 Rh1 130.2(2) .
C6 C1 Rh1 127.0(3) .
C3 C2 C1 108.7(2) .
C3 C2 C12 123.2(3) .
C1 C2 C12 128.1(3) .
C3 C2 Rh1 70.67(13) .
C1 C2 Rh1 69.51(15) .
C12 C2 Rh1 126.00(19) .
C2 C3 C4 108.3(2) .
C2 C3 C13 126.2(2) .
C4 C3 C13 125.5(2) .
C2 C3 Rh1 70.96(14) .
C4 C3 Rh1 69.40(12) .
C13 C3 Rh1 125.36(16) .
C5 C4 C3 107.6(2) .
C5 C4 C14 126.5(3) .
C3 C4 C14 125.8(2) .
C5 C4 Rh1 70.78(13) .
C3 C4 Rh1 71.10(12) .
C14 C4 Rh1 127.32(18) .
C4 C5 C1 108.4(2) .
C4 C5 C15 123.7(3) .
C1 C5 C15 127.8(3) .
C4 C5 Rh1 70.03(13) .
C1 C5 Rh1 70.10(14) .
C15 C5 Rh1 125.4(2) .
C11 C6 C7 103.3(13) .
C11 C6 C1 110.8(6) .
C7 C6 C1 103.3(15) .
C8 C7 C6 117(3) .
C7 C8 C9 109.5(16) .
C10 C9 C8 101.8(14) .
C11 C10 C9 116(3) .
C10 C11 C6 119.0(17) .
C11A C6A C1 111.9(4) .
C11A C6A C7A 108.4(11) .
C1 C6A C7A 102.7(10) .
C8A C7A C6A 114.9(17) .
C9A C8A C7A 117.9(11) .
C8A C9A C10A 115.8(13) .
C11A C10A C9A 115.5(19) .
C6A C11A C10A 110.1(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C4 2.127(2) .
Rh1 C1 2.132(2) .
Rh1 C5 2.137(2) .
Rh1 C3 2.149(2) .
Rh1 C2 2.153(2) .
Rh1 Cl1 2.3888(6) .
Rh1 Cl2 2.4473(6) .
Rh1 Cl2 2.4596(5) 3_656
Cl2 Rh1 2.4597(5) 3_656
C1 C5 1.441(5) .
C1 C2 1.444(5) .
C1 C6A 1.542(4) .
C1 C6 1.580(6) .
C2 C3 1.414(3) .
C2 C12 1.492(4) .
C3 C4 1.445(3) .
C3 C13 1.493(3) .
C4 C5 1.430(3) .
C4 C14 1.488(4) .
C5 C15 1.487(4) .
C6 C11 1.479(13) .
C6 C7 1.56(4) .
C7 C8 1.56(4) .
C8 C9 1.578(12) .
C9 C10 1.52(4) .
C10 C11 1.43(4) .
C6A C11A 1.526(9) .
C6A C7A 1.65(3) .
C7A C8A 1.48(3) .
C8A C9A 1.420(12) .
C9A C10A 1.59(3) .
C10A C11A 1.58(3) .
