#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:17:29 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178944 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/73/4117395.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_4117395
loop_
_publ_author_name
'Aaron Sattler'
'Gerard Parkin'
_publ_section_title
;
 A New Class of Transition Metal Pincer Ligand: Tantalum Complexes that
 Feature a [CCC] X3-Donor Array Derived from a Terphenyl Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2355
_journal_page_last               2366
_journal_paper_doi               10.1021/ja210404x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C26 H33 Cl2 P2 Ta'
_chemical_formula_weight         659.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 102.338(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4272(17)
_cell_length_b                   12.8506(18)
_cell_length_c                   16.636(2)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      31.99
_cell_measurement_theta_min      2.31
_cell_volume                     2595.4(6)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22162
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    4.577
_exptl_absorpt_correction_T_max  0.8035
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0281
_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)+(0.0266P)²+0.1067P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                3857
_reflns_number_total             4492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210404x_si_009.cif
_cod_data_source_block           pncl2s10
_cod_database_code               4117395
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ta Ta 0.5000 0.184769(11) 0.7500 0.02360(5) Uani 1 2 d S
P P 0.30451(6) 0.25601(6) 0.67536(4) 0.02758(14) Uani 1 1 d .
Cl Cl 0.37363(7) 0.04337(5) 0.75213(5) 0.04026(17) Uani 1 1 d .
C1 C 0.2102(2) 0.2620(3) 0.74454(19) 0.0374(7) Uani 1 1 d .
H1A H 0.2341 0.3165 0.7857 0.056 Uiso 1 1 calc R
H1B H 0.2095 0.1948 0.7722 0.056 Uiso 1 1 calc R
H1C H 0.1360 0.2780 0.7131 0.056 Uiso 1 1 calc R
C2 C 0.2821(2) 0.3824(2) 0.62596(18) 0.0332(6) Uani 1 1 d .
H2A H 0.2044 0.3893 0.5984 0.050 Uiso 1 1 calc R
H2B H 0.3283 0.3889 0.5853 0.050 Uiso 1 1 calc R
H2C H 0.3014 0.4372 0.6675 0.050 Uiso 1 1 calc R
C3 C 0.2387(3) 0.1705(2) 0.59197(19) 0.0388(7) Uani 1 1 d .
H3A H 0.1649 0.1969 0.5677 0.058 Uiso 1 1 calc R
H3B H 0.2328 0.1002 0.6135 0.058 Uiso 1 1 calc R
H3C H 0.2829 0.1683 0.5498 0.058 Uiso 1 1 calc R
C11 C 0.5000 0.3581(3) 0.7500 0.0237(7) Uani 1 2 d S
C12 C 0.5286(2) 0.4131(2) 0.68477(16) 0.0257(5) Uani 1 1 d .
C13 C 0.5296(2) 0.5218(2) 0.68567(19) 0.0330(6) Uani 1 1 d .
H13A H 0.5506 0.5591 0.6422 0.040 Uiso 1 1 calc R
C14 C 0.5000 0.5751(3) 0.7500 0.0365(9) Uani 1 2 d S
H14A H 0.5000 0.6490 0.7500 0.044 Uiso 1 2 calc SR
C21 C 0.5492(2) 0.3461(2) 0.61842(16) 0.0267(5) Uani 1 1 d .
C22 C 0.5335(2) 0.2392(2) 0.63195(16) 0.0267(5) Uani 1 1 d .
C23 C 0.5489(2) 0.1699(2) 0.57020(18) 0.0335(6) Uani 1 1 d .
H23A H 0.5384 0.0977 0.5780 0.040 Uiso 1 1 calc R
C24 C 0.5789(2) 0.2020(2) 0.49816(18) 0.0360(7) Uani 1 1 d .
C25 C 0.5956(2) 0.3076(2) 0.48870(18) 0.0363(7) Uani 1 1 d .
H25A H 0.6179 0.3313 0.4406 0.044 Uiso 1 1 calc R
C26 C 0.5808(2) 0.3795(2) 0.54735(17) 0.0327(6) Uani 1 1 d .
H26A H 0.5922 0.4515 0.5391 0.039 Uiso 1 1 calc R
C27 C 0.5954(3) 0.1239(3) 0.4341(2) 0.0489(8) Uani 1 1 d .
H27A H 0.6075 0.0548 0.4593 0.073 Uiso 1 1 calc R
H27B H 0.6595 0.1439 0.4121 0.073 Uiso 1 1 calc R
H27C H 0.5297 0.1223 0.3894 0.073 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'
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
C22 Ta C22 143.04(14) . 2_656
C22 Ta C11 71.52(7) . .
C22 Ta C11 71.52(7) 2_656 .
C22 Ta Cl 120.01(7) . .
C22 Ta Cl 88.76(7) 2_656 .
C11 Ta Cl 139.02(2) . .
C22 Ta Cl 88.76(7) . 2_656
C22 Ta Cl 120.01(7) 2_656 2_656
C11 Ta Cl 139.02(2) . 2_656
Cl Ta Cl 81.95(4) . 2_656
C22 Ta P 78.55(7) . .
C22 Ta P 88.80(7) 2_656 .
C11 Ta P 69.745(16) . .
Cl Ta P 74.42(3) . .
Cl Ta P 142.31(3) 2_656 .
C22 Ta P 88.80(7) . 2_656
C22 Ta P 78.55(7) 2_656 2_656
C11 Ta P 69.745(16) . 2_656
Cl Ta P 142.31(2) . 2_656
Cl Ta P 74.42(3) 2_656 2_656
P Ta P 139.49(3) . 2_656
C1 P C2 101.06(14) . .
C1 P C3 105.28(15) . .
C2 P C3 101.22(14) . .
C1 P Ta 111.76(11) . .
C2 P Ta 124.00(9) . .
C3 P Ta 111.52(11) . .
C12 C11 C12 119.5(3) 2_656 .
C12 C11 Ta 120.26(17) 2_656 .
C12 C11 Ta 120.26(17) . .
C13 C12 C11 119.9(3) . .
C13 C12 C21 126.4(2) . .
C11 C12 C21 113.6(2) . .
C14 C13 C12 120.0(3) . .
C13 C14 C13 120.7(4) 2_656 .
C26 C21 C22 120.7(3) . .
C26 C21 C12 125.8(3) . .
C22 C21 C12 113.5(2) . .
C23 C22 C21 117.1(2) . .
C23 C22 Ta 122.13(19) . .
C21 C22 Ta 120.61(19) . .
C24 C23 C22 123.1(3) . .
C25 C24 C23 117.5(3) . .
C25 C24 C27 121.6(3) . .
C23 C24 C27 120.8(3) . .
C26 C25 C24 121.8(3) . .
C25 C26 C21 119.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta C22 2.207(3) .
Ta C22 2.207(3) 2_656
Ta C11 2.227(4) .
Ta Cl 2.4069(7) .
Ta Cl 2.4069(7) 2_656
Ta P 2.6443(8) .
Ta P 2.6443(8) 2_656
P C1 1.811(3) .
P C2 1.815(3) .
P C3 1.821(3) .
C11 C12 1.403(3) 2_656
C11 C12 1.403(3) .
C12 C13 1.397(4) .
C12 C21 1.465(4) .
C13 C14 1.385(3) .
C14 C13 1.385(3) 2_656
C21 C26 1.391(4) .
C21 C22 1.412(4) .
C22 C23 1.403(4) .
C23 C24 1.391(4) .
C24 C25 1.388(4) .
C24 C27 1.509(4) .
C25 C26 1.384(4) .
