#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:48:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178724 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/35/4083593.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_4083593
loop_
_publ_author_name
'Mejuto, Carmen'
'Guisado-Barrios, Gregorio'
'Peris, Eduardo'
_publ_section_title
;
 Novel Rhodium and Iridium Complexes Coordinated toC3-Symmetric Tris-NHC
 Ligands Based on a 1,3,5-Triphenylbenzene Core. Electronic and Catalytic
 Properties
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3205
_journal_paper_doi               10.1021/om500547g
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         '4(C19 H24 Cl N2 Rh)'
_chemical_formula_sum            'C76 H96 Cl4 N8 Rh4'
_chemical_formula_weight         1675.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2908 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.886(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.1941(3)
_cell_length_b                   17.6476(4)
_cell_length_c                   10.3104(3)
_cell_measurement_reflns_used    16438
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.9010
_cell_measurement_theta_min      3.0380
_cell_volume                     1815.09(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9451
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0012253000
_diffrn_orient_matrix_UB_12      0.0046126000
_diffrn_orient_matrix_UB_13      0.0686187000
_diffrn_orient_matrix_UB_21      0.0359774000
_diffrn_orient_matrix_UB_22      0.0343991000
_diffrn_orient_matrix_UB_23      -0.0000854000
_diffrn_orient_matrix_UB_31      -0.0612590000
_diffrn_orient_matrix_UB_32      0.0202828000
_diffrn_orient_matrix_UB_33      -0.0154251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39071
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.42
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.5324
_exptl_crystal_description
;
;
_exptl_crystal_F_000             852.3407
_exptl_crystal_size_max          0.4043
_exptl_crystal_size_mid          0.1787
_exptl_crystal_size_min          0.1169
_refine_diff_density_max         0.7207
_refine_diff_density_min         -0.6314
_refine_diff_density_rms         0.1100
_refine_ls_d_res_high            0.7235
_refine_ls_d_res_low             7.2565
_refine_ls_goodness_of_fit_ref   1.0798
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0798
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0211P)²+1.3707P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -14
_reflns_number_gt                3975
_reflns_number_total             4737
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om500547g_si_001.cif
_cod_data_source_block           str1582
_cod_depositor_comments
'Adding full bibliography for 4083592--4083593.cif.'
_cod_original_cell_volume        1815.08(8)
_cod_database_code               4083593
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         'C H N Cl Rh'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_olex2_computing_structure_solution_long 'ShelXS-1997 (Sheldrick, 2008)'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z
3 -x,-y,-z
4 x-1/2,-y-1/2,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
Rh1 Rh 0.866860(15) 0.427505(9) 0.733082(16) 0.02114(6) Uani 1.000000
Cl1 Cl 0.86426(6) 0.55629(3) 0.66353(6) 0.03406(13) Uani 1.000000
C1 C 0.6655(2) 0.42525(11) 0.6693(2) 0.0224(4) Uani 1.000000
N5 N 0.59076(17) 0.39798(10) 0.55462(18) 0.0251(4) Uani 1.000000
N2 N 0.57457(18) 0.45264(11) 0.73595(19) 0.0284(4) Uani 1.000000
C7 C 0.8528(2) 0.33409(12) 0.8555(2) 0.0296(5) Uani 1.000000
C11 C 1.0819(2) 0.42023(13) 0.7362(3) 0.0322(5) Uani 1.000000
C16 C 0.6440(2) 0.36137(12) 0.4534(2) 0.0252(4) Uani 1.000000
C17 C 0.5841(2) 0.29563(13) 0.3959(2) 0.0319(5) Uani 1.000000
C6 C 0.8839(2) 0.30862(12) 0.7363(2) 0.0281(5) Uani 1.000000
C20 C 0.8069(2) 0.35418(15) 0.3164(3) 0.0364(5) Uani 1.000000
C19 C 0.7472(3) 0.28860(15) 0.2591(3) 0.0399(6) Uani 1.000000
C10 C 1.0678(2) 0.43530(13) 0.8627(3) 0.0340(5) Uani 1.000000
C21 C 0.7555(2) 0.39094(13) 0.4137(2) 0.0287(5) Uani 1.000000
C14 C 0.6092(3) 0.48917(15) 0.8662(2) 0.0367(5) Uani 1.000000
C13 C 1.0220(3) 0.28079(13) 0.7252(3) 0.0360(5) Uani 1.000000
C4 C 0.4545(2) 0.40868(14) 0.5510(3) 0.0319(5) Uani 1.000000
C18 C 0.6361(3) 0.25937(14) 0.2987(3) 0.0386(6) Uani 1.000000
C15 C 0.5768(3) 0.57279(16) 0.8590(3) 0.0423(6) Uani 1.000000
C12 C 1.1088(3) 0.34341(15) 0.6841(3) 0.0411(6) Uani 1.000000
C9 C 1.0846(3) 0.37745(16) 0.9732(3) 0.0421(6) Uani 1.000000
C8 C 0.9526(3) 0.34010(17) 0.9850(3) 0.0413(6) Uani 1.000000
C3 C 0.4454(2) 0.44228(14) 0.6639(3) 0.0348(5) Uani 1.000000
H18 H 0.6148(19) 0.2156(12) 0.2669(19) 0.008(5) Uiso 1.000000
H4 H 0.391(3) 0.3961(14) 0.479(3) 0.034(7) Uiso 1.000000
H17 H 0.508(3) 0.2770(14) 0.421(3) 0.037(7) Uiso 1.000000
H7 H 0.761(3) 0.3274(14) 0.865(2) 0.035(7) Uiso 1.000000
H13a H 1.015(2) 0.2422(15) 0.666(3) 0.034(7) Uiso 1.000000
H21 H 0.792(3) 0.4330(13) 0.453(3) 0.029(6) Uiso 1.000000
H14a H 0.563(3) 0.4611(15) 0.927(3) 0.040(7) Uiso 1.000000
H6 H 0.814(3) 0.2907(14) 0.671(3) 0.031(6) Uiso 1.000000
H12a H 1.090(3) 0.3458(15) 0.590(3) 0.037(7) Uiso 1.000000
H11 H 1.095(3) 0.4618(15) 0.684(3) 0.036(7) Uiso 1.000000
H10 H 1.067(2) 0.4849(15) 0.886(2) 0.031(6) Uiso 1.000000
H19 H 0.781(3) 0.2638(15) 0.193(3) 0.044(8) Uiso 1.000000
H9a H 1.149(2) 0.3384(14) 0.958(2) 0.033(7) Uiso 1.000000
H13b H 1.066(2) 0.2574(14) 0.808(3) 0.032(6) Uiso 1.000000
H8a H 0.912(3) 0.3683(16) 1.041(3) 0.045(8) Uiso 1.000000
H15a H 0.481(3) 0.5797(16) 0.827(3) 0.055(9) Uiso 1.000000
H15b H 0.604(3) 0.5944(16) 0.943(3) 0.045(8) Uiso 1.000000
H15c H 0.626(3) 0.5986(17) 0.798(3) 0.051(8) Uiso 1.000000
H14b H 0.700(3) 0.4816(14) 0.897(2) 0.035(7) Uiso 1.000000
H12b H 1.200(3) 0.3308(16) 0.712(3) 0.047(8) Uiso 1.000000
H20 H 0.883(3) 0.3753(16) 0.289(3) 0.046(8) Uiso 1.000000
H9b H 1.121(3) 0.4016(17) 1.054(3) 0.052(8) Uiso 1.000000
H3 H 0.374(3) 0.4601(17) 0.695(3) 0.047(8) Uiso 1.000000
H8b H 0.969(3) 0.2894(17) 1.024(3) 0.050(8) Uiso 1.000000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.14873 0.16029 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Rh -1.11611 0.93962 19.29570 14.35010 4.73425 1.28918 0.75154 8.21758 25.87490
98.60620 5.32800006866
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
14 0 -1 0.1784 14.0093 0.0039 -1.0031 -0.0516 0.5042 -0.8426
-1 -25 1 0.0799 -1.0089 -25.0036 0.9971 -0.0482 -0.8965 -0.4607
-13 -7 2 0.1738 -13.0116 -7.0054 2.0013 0.0891 -0.7093 0.6241
-1 25 -1 0.0985 -0.9923 25.0032 -0.9965 0.0457 0.8245 0.5833
0 -1 14 0.0548 -0.0118 -1.0161 13.9886 0.9552 -0.0366 -0.2357
0 1 -14 0.0621 0.0118 1.0161 -13.9886 -0.9552 0.0366 0.2357
6 15 -11 0.0785 6.0171 15.0151 -10.9913 -0.6776 0.7339 0.1055
12 9 -8 0.1149 12.0165 9.0123 -7.9960 -0.4924 0.7430 -0.4300
7 17 -9 0.0732 7.0167 17.0132 -8.9930 -0.5300 0.8384 0.0540
3 23 3 0.0915 3.0062 22.9992 2.9989 0.3156 0.8991 0.2361
1 -3 -14 0.0495 1.0112 -2.9840 -13.9892 -0.9724 -0.0651 0.0933
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Rh1 Cl1 88.47(6)
C7 Rh1 Cl1 158.84(7)
C7 Rh1 C1 89.42(8)
C11 Rh1 Cl1 90.53(6)
C11 Rh1 C1 161.71(10)
C11 Rh1 C7 97.89(9)
C6 Rh1 Cl1 162.12(7)
C6 Rh1 C1 93.47(8)
C6 Rh1 C7 39.04(9)
C6 Rh1 C11 82.08(9)
C10 Rh1 Cl1 94.25(6)
C10 Rh1 C1 161.99(10)
C10 Rh1 C7 81.63(9)
C10 Rh1 C11 36.25(10)
C10 Rh1 C6 89.38(9)
N5 C1 Rh1 129.84(15)
N2 C1 Rh1 125.71(15)
N2 C1 N5 104.45(17)
C16 N5 C1 124.66(17)
C4 N5 C1 110.65(19)
C4 N5 C16 124.66(19)
C14 N2 C1 124.19(19)
C3 N2 C1 110.9(2)
C3 N2 C14 124.9(2)
C6 C7 Rh1 70.70(12)
C8 C7 Rh1 111.13(16)
C8 C7 C6 124.4(2)
C10 C11 Rh1 72.59(13)
C12 C11 Rh1 107.66(16)
C12 C11 C10 125.3(2)
C17 C16 N5 119.44(19)
C21 C16 N5 120.25(19)
C21 C16 C17 120.3(2)
C18 C17 C16 119.7(2)
C7 C6 Rh1 70.26(12)
C13 C6 Rh1 113.34(15)
C13 C6 C7 123.3(2)
C21 C20 C19 120.2(2)
C18 C19 C20 120.2(2)
C11 C10 Rh1 71.16(13)
C9 C10 Rh1 111.16(16)
C9 C10 C11 124.7(2)
C20 C21 C16 119.5(2)
C15 C14 N2 112.1(2)
C12 C13 C6 112.69(19)
C3 C4 N5 106.6(2)
C19 C18 C17 120.1(2)
C13 C12 C11 113.2(2)
C8 C9 C10 112.7(2)
C9 C8 C7 113.9(2)
C4 C3 N2 107.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 Cl1 2.3817(6)
Rh1 C1 2.023(2)
Rh1 C7 2.099(2)
Rh1 C11 2.190(2)
Rh1 C6 2.105(2)
Rh1 C10 2.208(2)
C1 N5 1.356(3)
C1 N2 1.352(3)
N5 C16 1.426(3)
N5 C4 1.395(3)
N2 C14 1.465(3)
N2 C3 1.384(3)
C7 C6 1.405(3)
C7 C8 1.506(3)
C11 C10 1.368(4)
C11 C12 1.504(3)
C16 C17 1.386(3)
C16 C21 1.386(3)
C17 C18 1.384(4)
C6 C13 1.518(3)
C20 C19 1.383(4)
C20 C21 1.385(3)
C19 C18 1.380(4)
C10 C9 1.513(4)
C14 C15 1.511(4)
C13 C12 1.529(4)
C4 C3 1.327(4)
C9 C8 1.526(4)
