#------------------------------------------------------------------------------
#$Date: 2017-03-04 16:05:09 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193520 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/54/4125426.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_4125426
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         'C26 H42 Cl4 Rh2'
_chemical_formula_sum            'C26 H42 Cl4 Rh2'
_chemical_formula_weight         702.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.5113(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5293(7)
_cell_length_b                   10.5886(8)
_cell_length_c                   15.2966(12)
_cell_measurement_reflns_used    5043
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      2.69
_cell_volume                     1369.63(19)
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11564
_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         33.584
_diffrn_reflns_theta_min         2.346
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         5402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0385
_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)+(0.0314P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4100
_reflns_number_total             5402
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Rh11.cif
_cod_data_source_block           rovis188
_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               4125426
_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   0.683
_shelx_estimated_absorpt_t_max   0.865
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Rh1 Rh 0.07205(2) 0.93548(2) 0.11002(2) 0.01020(5) Uani 1 1 d . .
Cl1 Cl -0.18021(7) 0.96321(6) 0.01468(4) 0.01718(13) Uani 1 1 d . .
Cl2 Cl 0.03984(10) 1.13717(6) 0.17576(5) 0.02615(16) Uani 1 1 d . .
C1 C 0.0672(3) 0.8210(2) 0.22502(16) 0.0117(4) Uani 1 1 d . .
C2 C 0.0189(3) 0.7457(2) 0.14655(17) 0.0120(4) Uani 1 1 d . .
C3 C 0.1453(3) 0.7440(2) 0.09284(16) 0.0114(4) Uani 1 1 d . .
C4 C 0.2740(3) 0.8147(2) 0.13846(17) 0.0133(5) Uani 1 1 d . .
C5 C 0.2288(3) 0.8629(2) 0.21874(17) 0.0131(5) Uani 1 1 d . .
C6 C -0.0300(3) 0.8336(3) 0.30193(17) 0.0161(5) Uani 1 1 d . .
C7 C -0.0381(4) 0.7006(3) 0.3425(2) 0.0249(6) Uani 1 1 d . .
H7A H -0.1003 0.7041 0.3919 0.037 Uiso 1 1 calc R U
H7B H 0.0691 0.6712 0.3636 0.037 Uiso 1 1 calc R U
H7C H -0.0883 0.6422 0.2976 0.037 Uiso 1 1 calc R U
C8 C -0.1966(3) 0.8847(3) 0.2706(2) 0.0257(6) Uani 1 1 d . .
H8A H -0.2566 0.8904 0.3209 0.039 Uiso 1 1 calc R U
H8B H -0.2510 0.8275 0.2262 0.039 Uiso 1 1 calc R U
H8C H -0.1884 0.9687 0.2447 0.039 Uiso 1 1 calc R U
C9 C 0.0450(4) 0.9222(3) 0.3752(2) 0.0288(7) Uani 1 1 d . .
H9A H 0.0567 1.0067 0.3508 0.043 Uiso 1 1 calc R U
H9B H 0.1491 0.8897 0.3996 0.043 Uiso 1 1 calc R U
H9C H -0.0231 0.9267 0.4220 0.043 Uiso 1 1 calc R U
C10 C -0.1328(3) 0.6749(2) 0.11883(19) 0.0175(5) Uani 1 1 d . .
H10A H -0.2015 0.6815 0.1652 0.026 Uiso 1 1 calc R U
H10B H -0.1090 0.5858 0.1092 0.026 Uiso 1 1 calc R U
H10C H -0.1866 0.7113 0.0641 0.026 Uiso 1 1 calc R U
C11 C 0.1447(3) 0.6735(3) 0.00822(18) 0.0187(5) Uani 1 1 d . .
H11A H 0.2015 0.7225 -0.0320 0.028 Uiso 1 1 calc R U
H11B H 0.0353 0.6601 -0.0188 0.028 Uiso 1 1 calc R U
H11C H 0.1968 0.5916 0.0200 0.028 Uiso 1 1 calc R U
C12 C 0.4316(3) 0.8310(3) 0.10643(19) 0.0204(6) Uani 1 1 d . .
H12A H 0.4770 0.9126 0.1266 0.031 Uiso 1 1 calc R U
H12B H 0.4180 0.8282 0.0418 0.031 Uiso 1 1 calc R U
H12C H 0.5027 0.7629 0.1300 0.031 Uiso 1 1 calc R U
C13 C 0.3379(3) 0.9413(3) 0.28188(19) 0.0199(5) Uani 1 1 d . .
H13A H 0.3691 0.8931 0.3361 0.030 Uiso 1 1 calc R U
H13B H 0.2835 1.0188 0.2960 0.030 Uiso 1 1 calc R U
H13C H 0.4322 0.9632 0.2548 0.030 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
C5 Rh1 C1 40.00(9) .
C5 Rh1 C4 39.00(10) .
C1 Rh1 C4 66.24(10) .
C5 Rh1 C3 65.99(9) .
C1 Rh1 C3 66.63(9) .
C4 Rh1 C3 39.00(9) .
C5 Rh1 C2 65.98(9) .
C1 Rh1 C2 39.64(9) .
C4 Rh1 C2 65.22(9) .
C3 Rh1 C2 39.11(9) .
C5 Rh1 Cl2 95.08(7) .
C1 Rh1 Cl2 98.30(7) .
C4 Rh1 Cl2 125.50(7) .
C3 Rh1 Cl2 161.02(7) .
C2 Rh1 Cl2 133.29(7) .
C5 Rh1 Cl1 156.44(7) .
C1 Rh1 Cl1 116.51(7) .
C4 Rh1 Cl1 144.17(7) .
C3 Rh1 Cl1 106.66(7) .
C2 Rh1 Cl1 93.90(7) .
Cl2 Rh1 Cl1 90.18(3) .
C5 Rh1 Cl1 119.91(7) 3_575
C1 Rh1 Cl1 158.39(7) 3_575
C4 Rh1 Cl1 92.55(7) 3_575
C3 Rh1 Cl1 99.87(7) 3_575
C2 Rh1 Cl1 136.01(7) 3_575
Cl2 Rh1 Cl1 90.68(3) 3_575
Cl1 Rh1 Cl1 82.88(2) 3_575
Rh1 Cl1 Rh1 97.12(2) 3_575
C2 C1 C5 106.2(2) .
C2 C1 C6 124.0(2) .
C5 C1 C6 129.3(2) .
C2 C1 Rh1 70.49(14) .
C5 C1 Rh1 69.81(14) .
C6 C1 Rh1 130.76(17) .
C3 C2 C1 109.0(2) .
C3 C2 C10 120.9(2) .
C1 C2 C10 130.1(2) .
C3 C2 Rh1 70.37(13) .
C1 C2 Rh1 69.86(13) .
C10 C2 Rh1 126.45(17) .
C4 C3 C2 107.4(2) .
C4 C3 C11 126.8(2) .
C2 C3 C11 125.7(2) .
C4 C3 Rh1 70.37(14) .
C2 C3 Rh1 70.53(13) .
C11 C3 Rh1 127.58(18) .
C5 C4 C3 109.2(2) .
C5 C4 C12 126.5(2) .
C3 C4 C12 124.3(2) .
C5 C4 Rh1 70.20(14) .
C3 C4 Rh1 70.63(13) .
C12 C4 Rh1 126.57(19) .
C4 C5 C1 108.1(2) .
C4 C5 C13 122.4(2) .
C1 C5 C13 129.5(2) .
C4 C5 Rh1 70.80(14) .
C1 C5 Rh1 70.19(13) .
C13 C5 Rh1 125.03(18) .
C1 C6 C9 113.5(2) .
C1 C6 C8 111.2(2) .
C9 C6 C8 107.0(2) .
C1 C6 C7 106.7(2) .
C9 C6 C7 107.5(2) .
C8 C6 C7 111.0(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C5 2.136(2) .
Rh1 C1 2.141(2) .
Rh1 C4 2.144(2) .
Rh1 C3 2.147(2) .
Rh1 C2 2.150(2) .
Rh1 Cl2 2.3916(7) .
Rh1 Cl1 2.4540(6) .
Rh1 Cl1 2.4699(7) 3_575
Cl1 Rh1 2.4699(7) 3_575
C1 C2 1.455(3) .
C1 C5 1.463(3) .
C1 C6 1.531(4) .
C2 C3 1.438(3) .
C2 C10 1.508(3) .
C3 C4 1.433(3) .
C3 C11 1.494(4) .
C4 C5 1.429(4) .
C4 C12 1.499(4) .
C5 C13 1.501(4) .
C6 C9 1.536(4) .
C6 C8 1.538(4) .
C6 C7 1.543(4) .
