#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:28:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179503 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/00/4340075.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_4340075
loop_
_publ_author_name
'Barrett, Brittany J.'
'Iluc, Vlad M.'
_publ_section_title
;
 Coordination of a Hemilabile Pincer Ligand with an Olefinic Backbone to
 Mid-to-Late Transition Metals.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7248
_journal_page_last               7259
_journal_paper_doi               10.1021/ic500549z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C26 H38 Cl P2 Rh'
_chemical_formula_weight         550.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.3090(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8111(12)
_cell_length_b                   15.7865(16)
_cell_length_c                   14.7769(15)
_cell_measurement_temperature    120(2)
_cell_volume                     2584.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33562
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.9438
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0151P)²+9.0136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                4019
_reflns_number_total             5298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500549z_si_002.cif
_cod_data_source_block           bbrh1
_cod_depositor_comments
'Adding full bibliography for 4340069--4340078.cif.'
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4340075
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 1.0000 0.11661(3) 0.2500 0.01175(14) Uani 1 2 d S
C1 C 0.9984(5) 0.2415(3) 0.2980(3) 0.0127(7) Uani 1 1 d .
H1 H 1.0748 0.2602 0.3492 0.015 Uiso 1 1 calc R
Cl1 Cl 1.0000 -0.03324(11) 0.2500 0.0238(4) Uani 1 2 d S
P1 P 0.80459(12) 0.11676(8) 0.24626(9) 0.0153(3) Uani 1 1 d .
P2 P 0.68595(12) 0.69063(8) 0.23204(9) 0.0148(3) Uani 1 1 d .
Rh2 Rh 0.5000 0.69360(3) 0.2500 0.01198(14) Uani 1 2 d S
C2 C 0.4891(5) 0.5697(3) 0.1990(3) 0.0137(7) Uani 1 1 d .
H2 H 0.4060 0.5514 0.1581 0.016 Uiso 1 1 calc R
Cl2 Cl 0.5000 0.84302(11) 0.2500 0.0271(5) Uani 1 2 d S
C11 C 0.7793(4) 0.2242(3) 0.2778(3) 0.0151(11) Uani 1 1 d .
C12 C 0.8841(4) 0.2722(3) 0.3109(3) 0.0127(7) Uani 1 1 d .
C13 C 0.8807(5) 0.3518(3) 0.3516(3) 0.0190(11) Uani 1 1 d .
H13 H 0.9526 0.3842 0.3768 0.023 Uiso 1 1 calc R
C14 C 0.7732(5) 0.3834(3) 0.3551(3) 0.0237(12) Uani 1 1 d .
H14 H 0.7716 0.4373 0.3834 0.028 Uiso 1 1 calc R
C15 C 0.6679(5) 0.3370(3) 0.3178(4) 0.0234(12) Uani 1 1 d .
H15 H 0.5938 0.3596 0.3189 0.028 Uiso 1 1 calc R
C16 C 0.6706(5) 0.2583(3) 0.2792(3) 0.0206(12) Uani 1 1 d .
H16 H 0.5981 0.2267 0.2531 0.025 Uiso 1 1 calc R
C21 C 0.6962(5) 0.5845(3) 0.1886(3) 0.0164(11) Uani 1 1 d .
C22 C 0.5875(4) 0.5399(3) 0.1641(3) 0.0137(7) Uani 1 1 d .
C23 C 0.5752(5) 0.4642(3) 0.1121(3) 0.0207(12) Uani 1 1 d .
H23 H 0.5005 0.4347 0.0919 0.025 Uiso 1 1 calc R
C24 C 0.6715(5) 0.4325(3) 0.0902(4) 0.0250(13) Uani 1 1 d .
H24 H 0.6622 0.3815 0.0540 0.030 Uiso 1 1 calc R
C25 C 0.7810(5) 0.4738(3) 0.1201(4) 0.0279(13) Uani 1 1 d .
H25 H 0.8478 0.4496 0.1077 0.033 Uiso 1 1 calc R
C26 C 0.7943(5) 0.5504(3) 0.1682(4) 0.0233(12) Uani 1 1 d .
H26 H 0.8693 0.5796 0.1871 0.028 Uiso 1 1 calc R
C31 C 0.7862(5) 0.0516(3) 0.3442(4) 0.0212(12) Uani 1 1 d .
H31 H 0.8018 -0.0086 0.3307 0.025 Uiso 1 1 calc R
C32 C 0.6782(5) 0.0904(3) 0.1354(3) 0.0188(11) Uani 1 1 d .
H32 H 0.6016 0.1109 0.1425 0.023 Uiso 1 1 calc R
C33 C 0.8840(5) 0.0764(4) 0.4392(4) 0.0324(14) Uani 1 1 d .
H33A H 0.9636 0.0698 0.4332 0.049 Uiso 1 1 calc R
H33B H 0.8785 0.0398 0.4910 0.049 Uiso 1 1 calc R
H33C H 0.8725 0.1356 0.4542 0.049 Uiso 1 1 calc R
C34 C 0.6613(5) 0.0543(4) 0.3525(4) 0.0290(13) Uani 1 1 d .
H34A H 0.5998 0.0453 0.2887 0.043 Uiso 1 1 calc R
H34B H 0.6488 0.1096 0.3775 0.043 Uiso 1 1 calc R
H34C H 0.6550 0.0097 0.3966 0.043 Uiso 1 1 calc R
C35 C 0.6681(5) -0.0054(3) 0.1178(4) 0.0261(13) Uani 1 1 d .
H35A H 0.6063 -0.0170 0.0549 0.039 Uiso 1 1 calc R
H35B H 0.6455 -0.0328 0.1686 0.039 Uiso 1 1 calc R
H35C H 0.7460 -0.0276 0.1189 0.039 Uiso 1 1 calc R
C36 C 0.6964(5) 0.1374(3) 0.0511(4) 0.0256(13) Uani 1 1 d .
H36A H 0.6281 0.1259 -0.0082 0.038 Uiso 1 1 calc R
H36B H 0.7712 0.1179 0.0432 0.038 Uiso 1 1 calc R
H36C H 0.7017 0.1984 0.0642 0.038 Uiso 1 1 calc R
C41 C 0.8277(5) 0.7099(3) 0.3339(4) 0.0228(12) Uani 1 1 d .
H41 H 0.8971 0.6949 0.3130 0.027 Uiso 1 1 calc R
C42 C 0.6936(5) 0.7611(3) 0.1342(4) 0.0227(12) Uani 1 1 d .
H42 H 0.6800 0.8200 0.1531 0.027 Uiso 1 1 calc R
C43 C 0.8389(6) 0.8035(4) 0.3630(4) 0.0369(15) Uani 1 1 d .
H43A H 0.8477 0.8378 0.3106 0.055 Uiso 1 1 calc R
H43B H 0.9098 0.8113 0.4214 0.055 Uiso 1 1 calc R
H43C H 0.7663 0.8212 0.3757 0.055 Uiso 1 1 calc R
C44 C 0.8321(6) 0.6533(4) 0.4184(4) 0.0442(17) Uani 1 1 d .
H44A H 0.7637 0.6665 0.4391 0.066 Uiso 1 1 calc R
H44B H 0.9078 0.6630 0.4721 0.066 Uiso 1 1 calc R
H44C H 0.8276 0.5938 0.3985 0.066 Uiso 1 1 calc R
C45 C 0.8139(6) 0.7621(4) 0.1164(4) 0.0378(16) Uani 1 1 d .
H45A H 0.8274 0.7068 0.0919 0.057 Uiso 1 1 calc R
H45B H 0.8797 0.7742 0.1771 0.057 Uiso 1 1 calc R
H45C H 0.8116 0.8061 0.0690 0.057 Uiso 1 1 calc R
C46 C 0.5888(6) 0.7408(4) 0.0419(4) 0.0355(15) Uani 1 1 d .
H46A H 0.5852 0.7834 -0.0073 0.053 Uiso 1 1 calc R
H46B H 0.5131 0.7414 0.0551 0.053 Uiso 1 1 calc R
H46C H 0.6009 0.6846 0.0185 0.053 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'
P P 0.1023 0.0942 '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_1
_geom_angle_site_symmetry_3
C1 Rh1 C1 39.9(2) . 2_755
C1 Rh1 P1 96.80(14) . 2_755
C1 Rh1 P1 83.09(14) 2_755 2_755
C1 Rh1 P1 83.09(14) . .
C1 Rh1 P1 96.80(14) 2_755 .
P1 Rh1 P1 179.88(7) 2_755 .
C1 Rh1 Cl1 160.04(11) . .
C1 Rh1 Cl1 160.04(11) 2_755 .
P1 Rh1 Cl1 90.06(4) 2_755 .
P1 Rh1 Cl1 90.06(4) . .
C1 C1 C12 117.3(5) 2_755 .
C1 C1 Rh1 70.04(11) 2_755 .
C12 C1 Rh1 117.3(3) . .
C1 C1 H1 114.9 2_755 .
C12 C1 H1 114.9 . .
Rh1 C1 H1 114.9 . .
C11 P1 C32 106.6(2) . .
C11 P1 C31 104.2(2) . .
C32 P1 C31 106.9(2) . .
C11 P1 Rh1 104.47(17) . .
C32 P1 Rh1 121.36(16) . .
C31 P1 Rh1 111.83(17) . .
C21 P2 C41 106.7(2) . .
C21 P2 C42 104.6(2) . .
C41 P2 C42 105.2(2) . .
C21 P2 Rh2 104.08(17) . .
C41 P2 Rh2 122.25(17) . .
C42 P2 Rh2 112.63(18) . .
C2 Rh2 C2 40.4(2) . 2_655
C2 Rh2 P2 83.17(14) . .
C2 Rh2 P2 94.63(14) 2_655 .
C2 Rh2 P2 94.63(14) . 2_655
C2 Rh2 P2 83.17(14) 2_655 2_655
P2 Rh2 P2 177.67(7) . 2_655
C2 Rh2 Cl2 159.80(11) . .
C2 Rh2 Cl2 159.80(11) 2_655 .
P2 Rh2 Cl2 91.17(4) . .
P2 Rh2 Cl2 91.17(4) 2_655 .
C2 C2 C22 118.7(5) 2_655 .
C2 C2 Rh2 69.80(11) 2_655 .
C22 C2 Rh2 117.4(3) . .
C2 C2 H2 114.5 2_655 .
C22 C2 H2 114.5 . .
Rh2 C2 H2 114.5 . .
C12 C11 C16 119.7(4) . .
C12 C11 P1 113.3(4) . .
C16 C11 P1 126.8(4) . .
C11 C12 C13 119.2(5) . .
C11 C12 C1 120.5(4) . .
C13 C12 C1 120.2(4) . .
C14 C13 C12 120.3(5) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C15 C14 C13 120.3(5) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C16 C15 C14 119.9(5) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C11 120.6(5) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C22 C21 C26 120.3(4) . .
C22 C21 P2 112.9(4) . .
C26 C21 P2 126.3(4) . .
C21 C22 C23 118.8(4) . .
C21 C22 C2 120.3(4) . .
C23 C22 C2 120.7(4) . .
C24 C23 C22 120.1(5) . .
C24 C23 H23 119.9 . .
C22 C23 H23 119.9 . .
C25 C24 C23 120.7(5) . .
C25 C24 H24 119.6 . .
C23 C24 H24 119.6 . .
C24 C25 C26 120.4(5) . .
C24 C25 H25 119.8 . .
C26 C25 H25 119.8 . .
C25 C26 C21 119.4(5) . .
C25 C26 H26 120.3 . .
C21 C26 H26 120.3 . .
C34 C31 C33 111.3(4) . .
C34 C31 P1 115.3(4) . .
C33 C31 P1 108.7(4) . .
C34 C31 H31 107.1 . .
C33 C31 H31 107.1 . .
P1 C31 H31 107.1 . .
C36 C32 C35 111.5(4) . .
C36 C32 P1 108.4(3) . .
C35 C32 P1 111.4(4) . .
C36 C32 H32 108.5 . .
C35 C32 H32 108.5 . .
P1 C32 H32 108.5 . .
C31 C33 H33A 109.5 . .
C31 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C31 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C31 C34 H34A 109.5 . .
C31 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C31 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C32 C35 H35A 109.5 . .
C32 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C32 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C32 C36 H36A 109.5 . .
C32 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C32 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C44 C41 C43 111.2(5) . .
C44 C41 P2 109.6(4) . .
C43 C41 P2 110.7(4) . .
C44 C41 H41 108.4 . .
C43 C41 H41 108.4 . .
P2 C41 H41 108.4 . .
C46 C42 C45 111.2(4) . .
C46 C42 P2 109.2(4) . .
C45 C42 P2 116.1(4) . .
C46 C42 H42 106.6 . .
C45 C42 H42 106.6 . .
P2 C42 H42 106.6 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C41 C44 H44A 109.5 . .
C41 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C41 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C42 C45 H45A 109.5 . .
C42 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C42 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C42 C46 H46A 109.5 . .
C42 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C42 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C1 2.097(4) .
Rh1 C1 2.097(4) 2_755
Rh1 P1 2.2895(13) 2_755
Rh1 P1 2.2895(13) .
Rh1 Cl1 2.3656(18) .
C1 C1 1.432(8) 2_755
C1 C12 1.508(6) .
C1 H1 1.0000 .
P1 C11 1.811(5) .
P1 C32 1.841(5) .
P1 C31 1.848(5) .
P2 C21 1.813(5) .
P2 C41 1.848(5) .
P2 C42 1.850(5) .
P2 Rh2 2.3024(13) .
Rh2 C2 2.084(4) .
Rh2 C2 2.084(4) 2_655
Rh2 P2 2.3024(13) 2_655
Rh2 Cl2 2.3589(18) .
C2 C2 1.439(8) 2_655
C2 C22 1.502(6) .
C2 H2 1.0000 .
C11 C12 1.388(7) .
C11 C16 1.398(7) .
C12 C13 1.398(6) .
C13 C14 1.383(7) .
C13 H13 0.9500 .
C14 C15 1.382(8) .
C14 H14 0.9500 .
C15 C16 1.373(7) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.397(7) .
C21 C26 1.402(7) .
C22 C23 1.401(6) .
C23 C24 1.380(7) .
C23 H23 0.9500 .
C24 C25 1.377(8) .
C24 H24 0.9500 .
C25 C26 1.383(7) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C34 1.523(7) .
C31 C33 1.527(7) .
C31 H31 1.0000 .
C32 C36 1.528(6) .
C32 C35 1.532(7) .
C32 H32 1.0000 .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C41 C44 1.522(7) .
C41 C43 1.531(7) .
C41 H41 1.0000 .
C42 C46 1.524(8) .
C42 C45 1.532(7) .
C42 H42 1.0000 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
