#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:15:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178642 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/53/4075371.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_4075371
loop_
_publ_author_name
'Ma, Liqing'
'Woloszynek, Robert A.'
'Chen, Weizhong'
'Ren, Tong'
'Protasiewicz, John D.'
_publ_section_title
;
 A New Twist on Pincer Ligands and Complexes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3301
_journal_paper_doi               10.1021/om060256z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C42 H31 Br O2 P2 Pd'
_chemical_formula_weight         815.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9444(2)
_cell_length_b                   11.6289(2)
_cell_length_c                   19.7745(3)
_cell_measurement_reflns_used    2869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.62
_cell_measurement_theta_min      2.45
_cell_volume                     3436.55(9)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11657
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_type   'numerical face-indexed'
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'clear, light brown'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         6006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0349P)²+0.3357P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                4070
_reflns_number_total             6006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060256zsi20060321_102604.cif
_cod_data_source_block           case02
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4075371
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-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
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.0000 0.406272(19) 0.2500 0.01065(6) Uani 1 2 d S
Br1 Br 0.0000 0.19200(3) 0.2500 0.02436(8) Uani 1 2 d S
C1 C 0.0000 0.5837(3) 0.2500 0.0138(5) Uani 1 2 d S
C2 C -0.07079(14) 0.6461(2) 0.22133(10) 0.0154(4) Uani 1 1 d .
C3 C -0.07166(16) 0.7659(2) 0.22314(11) 0.0198(5) Uani 1 1 d .
H21 H -0.1219 0.8063 0.2058 0.027(7) Uiso 1 1 calc R
C4 C 0.0000 0.8271(3) 0.2500 0.0236(7) Uani 1 2 d S
H22 H 0.0000 0.9088 0.2500 0.019(10) Uiso 1 2 calc SR
C5 C -0.14434(14) 0.58696(19) 0.18517(10) 0.0147(4) Uani 1 1 d .
C6 C -0.23406(15) 0.5956(2) 0.20486(12) 0.0216(5) Uani 1 1 d .
H17 H -0.2493 0.6391 0.2438 0.019(7) Uiso 1 1 calc R
C7 C -0.30074(15) 0.5414(2) 0.16827(13) 0.0257(5) Uani 1 1 d .
H16 H -0.3612 0.5465 0.1828 0.041(8) Uiso 1 1 calc R
C8 C -0.27963(16) 0.4800(2) 0.11079(13) 0.0271(6) Uani 1 1 d .
H15 H -0.3258 0.4437 0.0856 0.023(7) Uiso 1 1 calc R
C9 C -0.19171(15) 0.4709(2) 0.08950(12) 0.0213(5) Uani 1 1 d .
H14 H -0.1770 0.4283 0.0500 0.030(8) Uiso 1 1 calc R
C10 C -0.12588(14) 0.5247(2) 0.12661(10) 0.0159(4) Uani 1 1 d .
O1 O -0.03735(10) 0.52142(13) 0.10293(7) 0.0144(3) Uani 1 1 d .
P1 P 0.02924(4) 0.42780(5) 0.13742(3) 0.01229(11) Uani 1 1 d .
C11 C 0.02395(15) 0.31342(19) 0.07515(10) 0.0141(4) Uani 1 1 d .
C12 C -0.04606(14) 0.2341(2) 0.07729(11) 0.0171(4) Uani 1 1 d .
H12 H -0.0853 0.2325 0.1150 0.016(6) Uiso 1 1 calc R
C13 C -0.05830(16) 0.1576(2) 0.02442(11) 0.0206(5) Uani 1 1 d .
H11 H -0.1066 0.1045 0.0258 0.020(7) Uiso 1 1 calc R
C14 C -0.00046(16) 0.1578(2) -0.03066(11) 0.0212(4) Uani 1 1 d .
H10 H -0.0084 0.1043 -0.0665 0.017(6) Uiso 1 1 calc R
C15 C 0.06875(16) 0.2366(2) -0.03285(11) 0.0194(5) Uani 1 1 d .
H9 H 0.1082 0.2375 -0.0705 0.035(8) Uiso 1 1 calc R
C16 C 0.08106(15) 0.31390(19) 0.01921(10) 0.0153(4) Uani 1 1 d .
H8 H 0.1287 0.3679 0.0170 0.012(6) Uiso 1 1 calc R
C17 C 0.13785(14) 0.4910(2) 0.12466(10) 0.0150(4) Uani 1 1 d .
C18 C 0.21127(14) 0.4285(2) 0.14746(11) 0.0196(5) Uani 1 1 d .
H2 H 0.2028 0.3564 0.1691 0.028(7) Uiso 1 1 calc R
C19 C 0.29732(15) 0.4721(2) 0.13848(12) 0.0246(5) Uani 1 1 d .
H3 H 0.3476 0.4292 0.1535 0.025(7) Uiso 1 1 calc R
C20 C 0.30960(16) 0.5774(2) 0.10787(12) 0.0248(5) Uani 1 1 d .
H4 H 0.3683 0.6069 0.1016 0.037(8) Uiso 1 1 calc R
C21 C 0.23617(16) 0.6404(2) 0.08627(12) 0.0247(5) Uani 1 1 d .
H5 H 0.2448 0.7134 0.0658 0.051(10) Uiso 1 1 calc R
C22 C 0.15014(15) 0.5976(2) 0.09438(11) 0.0196(5) Uani 1 1 d .
H6 H 0.1000 0.6409 0.0793 0.028(7) 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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 Pd1 P1 83.703(16) . 3
C1 Pd1 P1 83.703(16) . .
P1 Pd1 P1 167.41(3) 3 .
C1 Pd1 Br1 180.0 . .
P1 Pd1 Br1 96.297(16) 3 .
P1 Pd1 Br1 96.297(16) . .
C2 C1 C2 117.7(3) 3 .
C2 C1 Pd1 121.16(14) 3 .
C2 C1 Pd1 121.16(14) . .
C3 C2 C1 120.9(2) . .
C3 C2 C5 118.0(2) . .
C1 C2 C5 121.0(2) . .
C4 C3 C2 120.9(2) . .
C3 C4 C3 118.5(3) 3 .
C10 C5 C6 117.3(2) . .
C10 C5 C2 119.72(19) . .
C6 C5 C2 122.9(2) . .
C7 C6 C5 120.8(2) . .
C8 C7 C6 120.1(2) . .
C7 C8 C9 120.5(2) . .
C10 C9 C8 118.8(2) . .
C9 C10 C5 122.5(2) . .
C9 C10 O1 118.87(19) . .
C5 C10 O1 118.55(19) . .
C10 O1 P1 117.08(13) . .
O1 P1 C17 102.70(9) . .
O1 P1 C11 100.35(9) . .
C17 P1 C11 104.09(10) . .
O1 P1 Pd1 111.45(5) . .
C17 P1 Pd1 110.75(7) . .
C11 P1 Pd1 124.98(7) . .
C16 C11 C12 119.0(2) . .
C16 C11 P1 120.52(17) . .
C12 C11 P1 119.78(16) . .
C13 C12 C11 120.1(2) . .
C12 C13 C14 120.5(2) . .
C15 C14 C13 119.4(2) . .
C16 C15 C14 120.6(2) . .
C15 C16 C11 120.5(2) . .
C22 C17 C18 120.1(2) . .
C22 C17 P1 122.97(17) . .
C18 C17 P1 116.93(17) . .
C17 C18 C19 119.8(2) . .
C20 C19 C18 120.1(2) . .
C19 C20 C21 119.9(2) . .
C20 C21 C22 120.6(2) . .
C21 C22 C17 119.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 2.063(3) .
Pd1 P1 2.2824(5) 3
Pd1 P1 2.2824(5) .
Pd1 Br1 2.4918(4) .
C1 C2 1.403(3) 3
C1 C2 1.403(3) .
C2 C3 1.394(3) .
C2 C5 1.481(3) .
C3 C4 1.391(3) .
C4 C3 1.391(3) 3
C5 C10 1.393(3) .
C5 C6 1.400(3) .
C6 C7 1.383(3) .
C7 C8 1.379(4) .
C8 C9 1.384(3) .
C9 C10 1.378(3) .
C10 O1 1.404(2) .
O1 P1 1.6250(15) .
P1 C17 1.800(2) .
P1 C11 1.814(2) .
C11 C16 1.397(3) .
C11 C12 1.396(3) .
C12 C13 1.385(3) .
C13 C14 1.390(3) .
C14 C15 1.382(4) .
C15 C16 1.379(3) .
C17 C22 1.389(3) .
C17 C18 1.391(3) .
C18 C19 1.394(3) .
C19 C20 1.378(3) .
C20 C21 1.387(4) .
C21 C22 1.388(3) .
