#------------------------------------------------------------------------------
#$Date: 2017-03-04 16:05:09 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193520 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/54/4125421.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_4125421
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         'C18 H26 Cl4 Rh2'
_chemical_formula_sum            'C18 H26 Cl4 Rh2'
_chemical_formula_weight         590.01
_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                 101.2351(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9257(3)
_cell_length_b                   7.2269(3)
_cell_length_c                   16.0203(6)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.44
_cell_measurement_theta_min      2.59
_cell_volume                     1013.59(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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  0.0260
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22035
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.491
_diffrn_reflns_theta_min         2.433
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.070
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0196
_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)+(0.0409P)²+0.0923P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3525
_reflns_number_total             3895
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Rh14.cif
_cod_data_source_block           rovis222r
_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               4125421
_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   0.615
_shelx_estimated_absorpt_t_max   0.714
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 0.98943(2) 0.82386(2) 0.08009(2) 0.00782(5) Uani 1 1 d . .
Cl1 Cl 1.24851(5) 0.73947(7) 0.07805(3) 0.01330(9) Uani 1 1 d . .
Cl2 Cl 1.06162(5) 1.14918(6) 0.07573(3) 0.01077(8) Uani 1 1 d . .
C1 C 0.7602(2) 0.7288(3) 0.07970(12) 0.0122(3) Uani 1 1 d . .
C2 C 0.7970(2) 0.8784(3) 0.13834(12) 0.0114(3) Uani 1 1 d . .
C3 C 0.9275(2) 0.8241(2) 0.20256(12) 0.0110(3) Uani 1 1 d . .
C4 C 0.9706(2) 0.6396(3) 0.18302(12) 0.0112(3) Uani 1 1 d . .
C5 C 0.8702(2) 0.5827(3) 0.10609(12) 0.0118(3) Uani 1 1 d . .
H5 H 0.8751 0.4685 0.0774 0.014 Uiso 1 1 calc R U
C6 C 0.6320(2) 0.7252(3) 0.00445(13) 0.0177(4) Uani 1 1 d . .
H6A H 0.5357 0.7028 0.0234 0.027 Uiso 1 1 calc R U
H6B H 0.6495 0.6262 -0.0343 0.027 Uiso 1 1 calc R U
H6C H 0.6267 0.8444 -0.0252 0.027 Uiso 1 1 calc R U
C7 C 0.7138(2) 1.0591(3) 0.13409(14) 0.0183(4) Uani 1 1 d . .
H7A H 0.7032 1.1111 0.0767 0.028 Uiso 1 1 calc R U
H7B H 0.7714 1.1453 0.1755 0.028 Uiso 1 1 calc R U
H7C H 0.6122 1.0392 0.1472 0.028 Uiso 1 1 calc R U
C8 C 0.9970(2) 0.9379(3) 0.27779(12) 0.0160(4) Uani 1 1 d . .
H8A H 0.9285 0.9400 0.3187 0.024 Uiso 1 1 calc R U
H8B H 1.0130 1.0645 0.2594 0.024 Uiso 1 1 calc R U
H8C H 1.0954 0.8841 0.3048 0.024 Uiso 1 1 calc R U
C9 C 1.0986(2) 0.5271(3) 0.23226(13) 0.0162(4) Uani 1 1 d . .
H9A H 1.1792 0.6098 0.2612 0.024 Uiso 1 1 calc R U
H9B H 1.1399 0.4459 0.1933 0.024 Uiso 1 1 calc R U
H9C H 1.0604 0.4519 0.2745 0.024 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 C3 65.93(7) .
C5 Rh1 C2 65.87(7) .
C3 Rh1 C2 39.57(7) .
C5 Rh1 C4 39.22(7) .
C3 Rh1 C4 39.18(7) .
C2 Rh1 C4 65.88(7) .
C5 Rh1 C1 39.50(7) .
C3 Rh1 C1 65.70(7) .
C2 Rh1 C1 38.76(7) .
C4 Rh1 C1 65.75(7) .
C5 Rh1 Cl1 108.38(5) .
C3 Rh1 Cl1 115.77(5) .
C2 Rh1 Cl1 155.34(5) .
C4 Rh1 Cl1 94.17(5) .
C1 Rh1 Cl1 146.68(6) .
C5 Rh1 Cl2 160.05(5) .
C3 Rh1 Cl2 98.18(5) .
C2 Rh1 Cl2 94.23(5) .
C4 Rh1 Cl2 132.70(5) .
C1 Rh1 Cl2 124.19(6) .
Cl1 Rh1 Cl2 89.078(16) .
C5 Rh1 Cl2 105.27(5) 3_775
C3 Rh1 Cl2 154.42(5) 3_775
C2 Rh1 Cl2 114.95(5) 3_775
C4 Rh1 Cl2 143.25(5) 3_775
C1 Rh1 Cl2 91.96(5) 3_775
Cl1 Rh1 Cl2 89.699(16) 3_775
Cl2 Rh1 Cl2 83.818(16) 3_775
Rh1 Cl2 Rh1 96.182(16) 3_775
C2 C1 C5 107.71(16) .
C2 C1 C6 125.91(18) .
C5 C1 C6 126.38(18) .
C2 C1 Rh1 70.17(10) .
C5 C1 Rh1 69.06(10) .
C6 C1 Rh1 125.83(13) .
C1 C2 C3 108.17(16) .
C1 C2 C7 125.60(17) .
C3 C2 C7 126.23(17) .
C1 C2 Rh1 71.07(10) .
C3 C2 Rh1 70.00(10) .
C7 C2 Rh1 124.92(13) .
C4 C3 C2 107.95(16) .
C4 C3 C8 126.89(18) .
C2 C3 C8 125.07(17) .
C4 C3 Rh1 70.86(10) .
C2 C3 Rh1 70.43(10) .
C8 C3 Rh1 126.90(13) .
C5 C4 C3 107.67(16) .
C5 C4 C9 125.60(17) .
C3 C4 C9 126.72(18) .
C5 C4 Rh1 69.40(10) .
C3 C4 Rh1 69.96(10) .
C9 C4 Rh1 125.09(13) .
C4 C5 C1 108.44(16) .
C4 C5 Rh1 71.38(10) .
C1 C5 Rh1 71.44(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C5 2.1251(18) .
Rh1 C3 2.1394(18) .
Rh1 C2 2.1452(17) .
Rh1 C4 2.1514(18) .
Rh1 C1 2.1571(18) .
Rh1 Cl1 2.3979(4) .
Rh1 Cl2 2.4424(5) .
Rh1 Cl2 2.4564(5) 3_775
Cl2 Rh1 2.4564(5) 3_775
C1 C2 1.428(3) .
C1 C5 1.447(3) .
C1 C6 1.492(3) .
C2 C3 1.450(3) .
C2 C7 1.497(3) .
C3 C4 1.439(3) .
C3 C8 1.491(3) .
C4 C5 1.436(3) .
C4 C9 1.496(3) .
