#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:53:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179429 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/26/4332695.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332695
loop_
_publ_author_name
'Han, Hua'
'Elsmaili, Mona'
'Johnson, Samuel A.'
_publ_section_title
;
 Diligating Tripodal Amido-Phosphine Ligands:  the Effect of a
 Proximal Antipodal Early Transition Metal on Phosphine Donor Ability in a
 Building Block for Heterometallic Complexes
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7435
_journal_page_last               7445
_journal_paper_doi               10.1021/ic060692d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C63 H84 Cl N8 O P2 Rh Ta2'
_chemical_formula_weight         1531.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           176
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.2228(8)
_cell_length_b                   14.2228(8)
_cell_length_c                   25.594(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4483.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49687
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_T_max  0.7730
_exptl_absorpt_correction_T_min  0.6128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.731
_refine_diff_density_min         -2.796
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0572P)²+17.7139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                3116
_reflns_number_total             3513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060692dsup5.cif
_cod_data_source_block           hh135s
_cod_original_sg_symbol_H-M      P63/m
_cod_database_code               4332695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
C1 C 0.5378(4) 0.2252(4) 0.3671(2) 0.0303(10) Uani 1 1 d .
H1A H 0.4797 0.2409 0.3573 0.036 Uiso 1 1 calc R
H1B H 0.5207 0.1559 0.3501 0.036 Uiso 1 1 calc R
C2 C 0.4371(4) 0.1191(4) 0.4434(2) 0.0283(10) Uani 1 1 d .
C3 C 0.4397(4) 0.0858(4) 0.4945(2) 0.0296(10) Uani 1 1 d .
H3 H 0.5056 0.1198 0.5138 0.036 Uiso 1 1 calc R
C4 C 0.3453(4) 0.0024(4) 0.5172(2) 0.0318(11) Uani 1 1 d .
C5 C 0.2507(5) -0.0483(4) 0.4888(2) 0.0402(14) Uani 1 1 d .
H5 H 0.1868 -0.1051 0.5043 0.048 Uiso 1 1 calc R
C6 C 0.2478(4) -0.0174(5) 0.4383(3) 0.0422(14) Uani 1 1 d .
C7 C 0.3409(4) 0.0660(4) 0.4152(2) 0.0356(12) Uani 1 1 d .
H7 H 0.3387 0.0866 0.3801 0.043 Uiso 1 1 calc R
C8 C 0.3510(5) -0.0306(4) 0.5729(3) 0.0422(14) Uani 1 1 d .
H8A H 0.3765 0.0327 0.5959 0.063 Uiso 1 1 calc R
H8B H 0.4014 -0.0585 0.5747 0.063 Uiso 1 1 calc R
H8C H 0.2787 -0.0871 0.5841 0.063 Uiso 1 1 calc R
C9 C 0.1426(6) -0.0716(6) 0.4069(4) 0.075(3) Uani 1 1 d .
H9A H 0.1482 -0.1159 0.3791 0.112 Uiso 1 1 calc R
H9B H 0.1301 -0.0158 0.3914 0.112 Uiso 1 1 calc R
H9C H 0.0819 -0.1180 0.4300 0.112 Uiso 1 1 calc R
C10 C 0.6667 0.3333 0.5816(4) 0.040(2) Uani 1 3 d S
C11 C 0.7553(6) 0.4448(6) 0.6000(3) 0.0545(17) Uani 1 1 d .
H11A H 0.8261 0.4577 0.5878 0.082 Uiso 1 1 calc R
H11B H 0.7551 0.4475 0.6383 0.082 Uiso 1 1 calc R
H11C H 0.7416 0.5008 0.5858 0.082 Uiso 1 1 calc R
N1 N 0.5336(3) 0.2093(3) 0.42370(16) 0.0260(8) Uani 1 1 d .
N2 N 0.6667 0.3333 0.5244(3) 0.0293(15) Uani 1 3 d S
P1 P 0.6667 0.3333 0.33957(9) 0.0287(5) Uani 1 3 d S
Cl1 Cl 0.6406(8) 0.1684(5) 0.2500 0.057(2) Uani 0.33 2 d SP
Rh1 Rh 0.6667 0.3333 0.2500 0.0373(3) Uani 1 6 d S
Ta1 Ta 0.6667 0.3333 0.454552(13) 0.02345(13) Uani 1 3 d S
C12 C 0.787(2) 0.309(2) 0.2500 0.046(6) Uiso 0.33 2 d SP
O1 O 0.869(3) 0.281(3) 0.2500 0.119(12) Uiso 0.33 2 d SP
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'
Ta Ta -0.7052 6.5227 '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
N1 C1 P1 117.0(3) . .
C7 C2 C3 119.2(5) . .
C7 C2 N1 123.3(5) . .
C3 C2 N1 117.5(4) . .
C2 C3 C4 119.9(5) . .
C5 C4 C3 119.9(5) . .
C5 C4 C8 121.7(5) . .
C3 C4 C8 118.4(5) . .
C6 C5 C4 120.6(5) . .
C5 C6 C7 120.2(5) . .
C5 C6 C9 120.9(6) . .
C7 C6 C9 118.9(6) . .
C2 C7 C6 120.1(6) . .
N2 C10 C11 108.0(4) . 3_665
N2 C10 C11 108.0(4) . .
C11 C10 C11 110.9(4) 3_665 .
N2 C10 C11 108.0(4) . 2_655
C11 C10 C11 110.9(4) 3_665 2_655
C11 C10 C11 110.9(4) . 2_655
C2 N1 C1 116.0(4) . .
C2 N1 Ta1 135.9(3) . .
C1 N1 Ta1 107.9(3) . .
C10 N2 Ta1 180.000(2) . .
C1 P1 C1 106.33(19) 2_655 .
C1 P1 C1 106.33(19) 2_655 3_665
C1 P1 C1 106.33(19) . 3_665
C1 P1 Rh1 112.46(17) 2_655 .
C1 P1 Rh1 112.46(17) . .
C1 P1 Rh1 112.46(17) 3_665 .
C1 P1 Ta1 67.54(17) 2_655 .
C1 P1 Ta1 67.54(17) . .
C1 P1 Ta1 67.54(17) 3_665 .
Rh1 P1 Ta1 180.0 . .
C12 Cl1 C12 106.8(15) . 3_665
C12 Cl1 Rh1 53.6(8) . .
C12 Cl1 Rh1 53.2(8) 3_665 .
C12 Rh1 C12 120.000(3) . 3_665
C12 Rh1 C12 120.000(4) . 2_655
C12 Rh1 C12 120.000(3) 3_665 2_655
C12 Rh1 Cl1 59.5(9) . .
C12 Rh1 Cl1 60.5(9) 3_665 .
C12 Rh1 Cl1 179.5(9) 2_655 .
C12 Rh1 Cl1 60.5(9) . 2_655
C12 Rh1 Cl1 179.5(9) 3_665 2_655
C12 Rh1 Cl1 59.5(9) 2_655 2_655
Cl1 Rh1 Cl1 120.000(1) . 2_655
C12 Rh1 Cl1 179.5(9) . 3_665
C12 Rh1 Cl1 59.5(9) 3_665 3_665
C12 Rh1 Cl1 60.5(9) 2_655 3_665
Cl1 Rh1 Cl1 120.000(3) . 3_665
Cl1 Rh1 Cl1 120.000(1) 2_655 3_665
C12 Rh1 P1 90.000(1) . .
C12 Rh1 P1 90.000(2) 3_665 .
C12 Rh1 P1 90.000(1) 2_655 .
Cl1 Rh1 P1 90.0 . .
Cl1 Rh1 P1 90.0 2_655 .
Cl1 Rh1 P1 90.0 3_665 .
C12 Rh1 P1 90.000(1) . 10_556
C12 Rh1 P1 90.000(2) 3_665 10_556
C12 Rh1 P1 90.000(1) 2_655 10_556
Cl1 Rh1 P1 90.0 . 10_556
Cl1 Rh1 P1 90.0 2_655 10_556
Cl1 Rh1 P1 90.0 3_665 10_556
P1 Rh1 P1 180.0 . 10_556
N2 Ta1 N1 113.32(12) . 2_655
N2 Ta1 N1 113.32(12) . .
N1 Ta1 N1 105.37(13) 2_655 .
N2 Ta1 N1 113.32(12) . 3_665
N1 Ta1 N1 105.37(13) 2_655 3_665
N1 Ta1 N1 105.37(13) . 3_665
N2 Ta1 P1 180.000(1) . .
N1 Ta1 P1 66.68(12) 2_655 .
N1 Ta1 P1 66.68(12) . .
N1 Ta1 P1 66.68(12) 3_665 .
O1 C12 Rh1 175(3) . .
O1 C12 Cl1 108(2) . .
Rh1 C12 Cl1 66.9(9) . .
O1 C12 Cl1 119(2) . 2_655
Rh1 C12 Cl1 66.3(9) . 2_655
Cl1 C12 Cl1 133.2(15) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.463(7) .
C1 P1 1.844(5) .
C2 C7 1.390(8) .
C2 C3 1.397(7) .
C2 N1 1.422(6) .
C3 C4 1.398(7) .
C4 C5 1.373(8) .
C4 C8 1.517(8) .
C5 C6 1.373(9) .
C6 C7 1.392(8) .
C6 C9 1.524(9) .
C10 N2 1.464(12) .
C10 C11 1.525(8) 3_665
C10 C11 1.525(8) .
C10 C11 1.525(8) 2_655
N1 Ta1 1.995(4) .
N2 Ta1 1.787(9) .
P1 C1 1.844(5) 2_655
P1 C1 1.844(5) 3_665
P1 Rh1 2.292(2) .
P1 Ta1 2.943(2) .
Cl1 C12 2.05(3) .
Cl1 C12 2.08(3) 3_665
Cl1 Rh1 2.184(6) .
Rh1 C12 1.91(3) .
Rh1 C12 1.91(3) 3_665
Rh1 C12 1.91(3) 2_655
Rh1 Cl1 2.184(6) 2_655
Rh1 Cl1 2.184(6) 3_665
Rh1 P1 2.292(2) 10_556
Ta1 N1 1.995(4) 2_655
Ta1 N1 1.995(4) 3_665
C12 O1 1.40(5) .
C12 Cl1 2.08(3) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 42.7 18.2
2 -0.017 -0.012 0.250 733.6 311.9
3 0.000 0.000 0.500 42.6 17.2
4 -0.016 -0.014 0.750 733.5 309.6
