#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329614.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_4329614
loop_
_publ_author_name
'Thomas S. Teets'
'Daniel G. Nocera'
_publ_section_title
;
 Oxygen Reduction Reactions of Monometallic Rhodium Hydride Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7192
_journal_page_last               7201
_journal_paper_doi               10.1021/ic300279z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C21 H39 Cl N O2 P2 Rh'
_chemical_formula_weight         537.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.796(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.214(2)
_cell_length_b                   11.4156(18)
_cell_length_c                   15.778(3)
_cell_measurement_reflns_used    9298
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.27
_cell_volume                     2507.3(7)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57744
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.8356
_exptl_absorpt_correction_T_min  0.8005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0181P)²+1.4523P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                6695
_reflns_number_total             7671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300279z_si_002_3.cif
_cod_data_source_block           4b
_cod_database_code               4329614
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.409799(6) 0.752133(7) 0.212434(6) 0.01096(3) Uani 1 1 d .
P1 P 0.39576(2) 0.75739(2) 0.05982(2) 0.01396(6) Uani 1 1 d .
P2 P 0.40553(2) 0.75561(2) 0.35862(2) 0.01228(5) Uani 1 1 d .
Cl1 Cl 0.56630(2) 0.84753(3) 0.26856(2) 0.01922(6) Uani 1 1 d .
O1 O 0.29930(6) 0.86992(7) 0.16919(6) 0.01838(16) Uani 1 1 d .
O2 O 0.26621(6) 0.75066(7) 0.16318(6) 0.01785(17) Uani 1 1 d .
N1 N 0.51146(7) 0.51157(8) 0.25036(7) 0.01647(18) Uani 1 1 d .
C1 C 0.47262(8) 0.60176(10) 0.23622(8) 0.0146(2) Uani 1 1 d .
C2 C 0.56368(8) 0.40711(10) 0.27436(8) 0.0146(2) Uani 1 1 d .
C3 C 0.65930(9) 0.40824(12) 0.28419(9) 0.0212(2) Uani 1 1 d .
C4 C 0.70921(10) 0.30233(15) 0.30677(10) 0.0315(3) Uani 1 1 d .
H4 H 0.7743 0.2993 0.3140 0.038 Uiso 1 1 calc R
C5 C 0.66487(12) 0.20162(14) 0.31880(11) 0.0338(3) Uani 1 1 d .
H5 H 0.7003 0.1305 0.3350 0.041 Uiso 1 1 calc R
C6 C 0.57004(11) 0.20279(11) 0.30760(10) 0.0263(3) Uani 1 1 d .
H6 H 0.5409 0.1324 0.3155 0.032 Uiso 1 1 calc R
C7 C 0.51661(9) 0.30609(10) 0.28475(8) 0.0175(2) Uani 1 1 d .
C8 C 0.70389(10) 0.51763(15) 0.26652(10) 0.0325(3) Uani 1 1 d .
H8A H 0.6723 0.5385 0.2008 0.049 Uiso 1 1 calc R
H8B H 0.7724 0.5042 0.2829 0.049 Uiso 1 1 calc R
H8C H 0.6961 0.5817 0.3043 0.049 Uiso 1 1 calc R
C9 C 0.41252(10) 0.30944(13) 0.26908(11) 0.0280(3) Uani 1 1 d .
H9A H 0.3927 0.2319 0.2814 0.042 Uiso 1 1 calc R
H9B H 0.3736 0.3316 0.2047 0.042 Uiso 1 1 calc R
H9C H 0.4033 0.3670 0.3109 0.042 Uiso 1 1 calc R
C11 C 0.50267(9) 0.70969(12) 0.04359(9) 0.0205(2) Uani 1 1 d .
H11A H 0.5537 0.7689 0.0721 0.025 Uiso 1 1 calc R
H11B H 0.5254 0.6355 0.0779 0.025 Uiso 1 1 calc R
C12 C 0.49047(11) 0.69049(13) -0.05652(9) 0.0264(3) Uani 1 1 d .
H12A H 0.4487 0.6228 -0.0825 0.040 Uiso 1 1 calc R
H12B H 0.5534 0.6761 -0.0578 0.040 Uiso 1 1 calc R
H12C H 0.4615 0.7603 -0.0933 0.040 Uiso 1 1 calc R
C21 C 0.29505(9) 0.67144(12) -0.01918(9) 0.0229(2) Uani 1 1 d .
H21A H 0.2347 0.7040 -0.0192 0.027 Uiso 1 1 calc R
H21B H 0.2923 0.6798 -0.0827 0.027 Uiso 1 1 calc R
C22 C 0.30020(12) 0.54177(13) 0.00467(11) 0.0337(3) Uani 1 1 d .
H22A H 0.3561 0.5067 -0.0015 0.051 Uiso 1 1 calc R
H22B H 0.2416 0.5026 -0.0377 0.051 Uiso 1 1 calc R
H22C H 0.3062 0.5325 0.0685 0.051 Uiso 1 1 calc R
C31 C 0.36721(9) 0.90284(11) 0.00684(9) 0.0210(2) Uani 1 1 d .
H31A H 0.3762 0.9015 -0.0519 0.025 Uiso 1 1 calc R
H31B H 0.2985 0.9192 -0.0088 0.025 Uiso 1 1 calc R
C32 C 0.42672(10) 1.00314(11) 0.06651(10) 0.0263(3) Uani 1 1 d .
H32A H 0.4150 1.0092 0.1230 0.039 Uiso 1 1 calc R
H32B H 0.4083 1.0767 0.0317 0.039 Uiso 1 1 calc R
H32C H 0.4951 0.9880 0.0831 0.039 Uiso 1 1 calc R
C41 C 0.33240(9) 0.63493(10) 0.37050(8) 0.0169(2) Uani 1 1 d .
H41A H 0.2722 0.6322 0.3137 0.020 Uiso 1 1 calc R
H41B H 0.3673 0.5609 0.3733 0.020 Uiso 1 1 calc R
C42 C 0.30574(10) 0.63872(12) 0.45414(10) 0.0253(3) Uani 1 1 d .
H42A H 0.3644 0.6435 0.5112 0.038 Uiso 1 1 calc R
H42B H 0.2702 0.5676 0.4553 0.038 Uiso 1 1 calc R
H42C H 0.2655 0.7075 0.4495 0.038 Uiso 1 1 calc R
C51 C 0.34746(9) 0.88829(10) 0.37517(9) 0.0188(2) Uani 1 1 d .
H51A H 0.2800 0.8892 0.3291 0.023 Uiso 1 1 calc R
H51B H 0.3466 0.8860 0.4375 0.023 Uiso 1 1 calc R
C52 C 0.39649(10) 1.00143(10) 0.36571(9) 0.0221(2) Uani 1 1 d .
H52A H 0.4620 1.0040 0.4139 0.033 Uiso 1 1 calc R
H52B H 0.3601 1.0689 0.3726 0.033 Uiso 1 1 calc R
H52C H 0.3988 1.0039 0.3046 0.033 Uiso 1 1 calc R
C61 C 0.51879(9) 0.75004(10) 0.46143(8) 0.0175(2) Uani 1 1 d .
H61A H 0.5579 0.8192 0.4610 0.021 Uiso 1 1 calc R
H61B H 0.5045 0.7557 0.5172 0.021 Uiso 1 1 calc R
C62 C 0.57833(9) 0.63982(11) 0.46907(9) 0.0217(2) Uani 1 1 d .
H62A H 0.5395 0.5705 0.4667 0.033 Uiso 1 1 calc R
H62B H 0.6351 0.6408 0.5279 0.033 Uiso 1 1 calc R
H62C H 0.5986 0.6374 0.4175 0.033 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
C1 Rh1 O2 116.49(4)
C1 Rh1 O1 158.15(4)
O2 Rh1 O1 41.74(3)
C1 Rh1 P1 93.19(3)
O2 Rh1 P1 88.19(3)
O1 Rh1 P1 85.29(3)
C1 Rh1 P2 91.84(3)
O2 Rh1 P2 85.56(3)
O1 Rh1 P2 88.37(3)
P1 Rh1 P2 173.268(11)
C1 Rh1 Cl1 89.55(4)
O2 Rh1 Cl1 153.92(2)
O1 Rh1 Cl1 112.27(3)
P1 Rh1 Cl1 91.876(11)
P2 Rh1 Cl1 92.634(12)
C21 P1 C11 107.08(6)
C21 P1 C31 101.35(6)
C11 P1 C31 105.47(6)
C21 P1 Rh1 113.20(4)
C11 P1 Rh1 114.90(4)
C31 P1 Rh1 113.64(4)
C51 P2 C41 105.14(6)
C51 P2 C61 103.84(6)
C41 P2 C61 106.11(6)
C51 P2 Rh1 111.33(4)
C41 P2 Rh1 110.45(4)
C61 P2 Rh1 118.93(4)
O2 O1 Rh1 67.59(5)
O1 O2 Rh1 70.67(5)
C1 N1 C2 175.18(12)
N1 C1 Rh1 179.16(10)
N1 C2 C3 118.29(11)
N1 C2 C7 118.17(10)
C3 C2 C7 123.51(11)
C4 C3 C2 117.04(12)
C4 C3 C8 121.90(13)
C2 C3 C8 120.99(12)
C5 C4 C3 120.63(13)
C6 C5 C4 121.08(12)
C5 C6 C7 120.74(13)
C6 C7 C2 116.99(12)
C6 C7 C9 122.02(12)
C2 C7 C9 120.97(11)
C12 C11 P1 116.30(9)
C22 C21 P1 114.16(10)
C32 C31 P1 115.24(9)
C42 C41 P2 116.84(9)
C52 C51 P2 113.82(9)
C62 C61 P2 114.53(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 C1 1.9265(12)
Rh1 O2 2.0016(9)
Rh1 O1 2.0430(8)
Rh1 P1 2.3307(5)
Rh1 P2 2.3339(5)
Rh1 Cl1 2.4367(4)
P1 C21 1.8230(13)
P1 C11 1.8286(13)
P1 C31 1.8306(13)
P2 C51 1.8246(12)
P2 C41 1.8274(12)
P2 C61 1.8300(13)
O1 O2 1.4413(12)
N1 C1 1.1630(15)
N1 C2 1.3978(14)
C2 C3 1.3994(17)
C2 C7 1.4016(16)
C3 C4 1.3953(19)
C3 C8 1.4999(19)
C4 C5 1.384(2)
C5 C6 1.381(2)
C6 C7 1.3947(17)
C7 C9 1.5014(18)
C11 C12 1.5301(17)
C21 C22 1.522(2)
C31 C32 1.5261(19)
C41 C42 1.5297(17)
C51 C52 1.5286(17)
C61 C62 1.5264(17)
