#------------------------------------------------------------------------------
#$Date: 2019-11-28 19:42:27 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244425 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/07/4350756.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_4350756
loop_
_publ_author_name
'Adhikary, Anubendu'
'Schwartz, Jason R.'
'Meadows, Lonnie M.'
'Krause, Jeanette A.'
'Guan, Hairong'
_publ_section_title
;
 Interaction of alkynes with palladium POCOP-pincer hydride complexes and
 its unexpected relation to palladium-catalyzed hydrogenation of alkynes
;
_journal_issue                   1
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              71
_journal_paper_doi               10.1039/C3QI00073G
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C26 H38 O2 P2 Pd'
_chemical_formula_sum            'C26 H38 O2 P2 Pd'
_chemical_formula_weight         550.90
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 101.659(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8023(2)
_cell_length_b                   14.4839(4)
_cell_length_c                   12.0669(3)
_cell_measurement_reflns_used    7155
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.87
_cell_measurement_theta_min      3.05
_cell_volume                     1335.52(6)
_computing_cell_refinement       'Bruker SAINT v7.66A'
_computing_data_collection       'Bruker SMART v5.634'
_computing_data_reduction        'Bruker SAINT v7.66A'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART6000 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10793
_diffrn_reflns_theta_full        67.28
_diffrn_reflns_theta_max         67.28
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    6.878
_exptl_absorpt_correction_T_max  0.3707
_exptl_absorpt_correction_T_min  0.3261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0273
_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)+(0.0480P)²+0.3075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                2219
_reflns_number_total             2453
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3qi00073g.txt
_cod_data_source_block           4B
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4350756
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
Pd Pd 0.24755(3) 0.2500 0.758012(18) 0.02528(11) Uani 1 2 d S
P1 P 0.28122(8) 0.09681(5) 0.73679(5) 0.02888(16) Uani 1 1 d .
O1 O 0.3707(3) 0.08481(13) 0.62374(15) 0.0416(5) Uani 1 1 d .
C1 C 0.3700(4) 0.2500 0.6246(3) 0.0330(8) Uani 1 2 d S
C2 C 0.4178(3) 0.1680(2) 0.5794(2) 0.0386(7) Uani 1 1 d .
C3 C 0.5090(4) 0.1661(2) 0.4911(2) 0.0498(8) Uani 1 1 d .
H3 H 0.5404 0.1094 0.4609 0.060 Uiso 1 1 calc R
C4 C 0.5518(5) 0.2500 0.4493(3) 0.0547(13) Uani 1 2 d S
H4 H 0.6135 0.2500 0.3890 0.066 Uiso 1 2 calc SR
C7 C 0.4434(3) 0.04006(17) 0.8462(2) 0.0321(5) Uani 1 1 d .
H7 H 0.3898 0.0323 0.9143 0.039 Uiso 1 1 calc R
C8 C 0.6025(3) 0.1035(2) 0.8799(2) 0.0411(6) Uani 1 1 d .
H8A H 0.6903 0.0732 0.9381 0.062 Uiso 1 1 calc R
H8B H 0.5661 0.1616 0.9099 0.062 Uiso 1 1 calc R
H8C H 0.6528 0.1163 0.8134 0.062 Uiso 1 1 calc R
C9 C 0.4966(4) -0.05535(19) 0.8124(2) 0.0433(7) Uani 1 1 d .
H9A H 0.5801 -0.0827 0.8754 0.065 Uiso 1 1 calc R
H9B H 0.5513 -0.0500 0.7463 0.065 Uiso 1 1 calc R
H9C H 0.3927 -0.0948 0.7935 0.065 Uiso 1 1 calc R
C10 C 0.0918(3) 0.02041(19) 0.7029(2) 0.0419(7) Uani 1 1 d .
H10 H 0.1282 -0.0380 0.6699 0.050 Uiso 1 1 calc R
C11 C -0.0498(4) 0.0679(2) 0.6137(3) 0.0625(10) Uani 1 1 d .
H11A H -0.1466 0.0248 0.5882 0.094 Uiso 1 1 calc R
H11B H 0.0005 0.0865 0.5490 0.094 Uiso 1 1 calc R
H11C H -0.0935 0.1225 0.6470 0.094 Uiso 1 1 calc R
C12 C 0.0248(4) -0.0033(2) 0.8099(3) 0.0495(7) Uani 1 1 d .
H12A H -0.0868 -0.0363 0.7892 0.074 Uiso 1 1 calc R
H12B H 0.0077 0.0537 0.8501 0.074 Uiso 1 1 calc R
H12C H 0.1105 -0.0425 0.8590 0.074 Uiso 1 1 calc R
C27 C 0.1237(4) 0.2500 0.8940(3) 0.0267(7) Uani 1 2 d S
H27 H -0.0006 0.2500 0.8752 0.032 Uiso 1 2 calc SR
C28 C 0.1931(4) 0.2500 1.0041(3) 0.0262(7) Uani 1 2 d S
H28 H 0.3173 0.2500 1.0236 0.031 Uiso 1 2 calc SR
C29 C 0.1012(4) 0.2500 1.1001(3) 0.0262(7) Uani 1 2 d S
C30 C 0.1971(4) 0.2500 1.2116(3) 0.0283(7) Uani 1 2 d S
H30 H 0.3213 0.2500 1.2246 0.034 Uiso 1 2 calc SR
C31 C 0.1150(5) 0.2500 1.3033(3) 0.0349(8) Uani 1 2 d S
H31 H 0.1829 0.2500 1.3781 0.042 Uiso 1 2 calc SR
C32 C -0.0654(5) 0.2500 1.2857(3) 0.0398(9) Uani 1 2 d S
H32 H -0.1221 0.2500 1.3484 0.048 Uiso 1 2 calc SR
C33 C -0.1631(5) 0.2500 1.1766(3) 0.0381(9) Uani 1 2 d S
H33 H -0.2872 0.2500 1.1644 0.046 Uiso 1 2 calc SR
C34 C -0.0814(4) 0.2500 1.0849(3) 0.0300(7) Uani 1 2 d S
H34 H -0.1505 0.2500 1.0105 0.036 Uiso 1 2 calc SR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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 Pd C27 179.84(12) . .
C1 Pd P1 79.964(18) . 4_565
C27 Pd P1 100.030(18) . 4_565
C1 Pd P1 79.964(18) . .
C27 Pd P1 100.030(18) . .
P1 Pd P1 159.45(3) 4_565 .
O1 P1 C10 101.99(12) . .
O1 P1 C7 101.65(10) . .
C10 P1 C7 107.45(13) . .
O1 P1 Pd 105.90(7) . .
C10 P1 Pd 120.96(9) . .
C7 P1 Pd 116.08(8) . .
C2 O1 P1 114.24(16) . .
C2 C1 C2 117.6(3) . 4_565
C2 C1 Pd 121.18(16) . .
C2 C1 Pd 121.18(16) 4_565 .
C1 C2 C3 122.4(3) . .
C1 C2 O1 118.3(2) . .
C3 C2 O1 119.3(3) . .
C4 C3 C2 117.3(3) . .
C4 C3 H3 121.3 . .
C2 C3 H3 121.3 . .
C3 C4 C3 123.1(4) 4_565 .
C3 C4 H4 118.5 4_565 .
C3 C4 H4 118.5 . .
C9 C7 C8 111.4(2) . .
C9 C7 P1 113.60(18) . .
C8 C7 P1 109.10(18) . .
C9 C7 H7 107.5 . .
C8 C7 H7 107.5 . .
P1 C7 H7 107.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C12 C10 C11 111.8(3) . .
C12 C10 P1 110.30(18) . .
C11 C10 P1 108.7(2) . .
C12 C10 H10 108.7 . .
C11 C10 H10 108.7 . .
P1 C10 H10 108.7 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C28 C27 Pd 129.2(3) . .
C28 C27 H27 115.4 . .
Pd C27 H27 115.4 . .
C27 C28 C29 128.2(3) . .
C27 C28 H28 115.9 . .
C29 C28 H28 115.9 . .
C34 C29 C30 117.2(3) . .
C34 C29 C28 122.6(3) . .
C30 C29 C28 120.2(3) . .
C31 C30 C29 121.6(3) . .
C31 C30 H30 119.2 . .
C29 C30 H30 119.2 . .
C32 C31 C30 119.9(3) . .
C32 C31 H31 120.0 . .
C30 C31 H31 120.0 . .
C31 C32 C33 119.7(3) . .
C31 C32 H32 120.2 . .
C33 C32 H32 120.2 . .
C32 C33 C34 120.5(3) . .
C32 C33 H33 119.8 . .
C34 C33 H33 119.8 . .
C33 C34 C29 121.1(3) . .
C33 C34 H34 119.4 . .
C29 C34 H34 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd C1 2.031(3) .
Pd C27 2.066(3) .
Pd P1 2.2549(6) 4_565
Pd P1 2.2549(6) .
P1 O1 1.6622(18) .
P1 C10 1.825(3) .
P1 C7 1.829(2) .
O1 C2 1.397(3) .
C1 C2 1.389(3) .
C1 C2 1.389(3) 4_565
C2 C3 1.396(4) .
C3 C4 1.382(4) .
C3 H3 0.9500 .
C4 C3 1.382(4) 4_565
C4 H4 0.9500 .
C7 C9 1.523(4) .
C7 C8 1.532(4) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C12 1.527(4) .
C10 C11 1.540(4) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C27 C28 1.329(5) .
C27 H27 0.9500 .
C28 C29 1.480(4) .
C28 H28 0.9500 .
C29 C34 1.400(5) .
C29 C30 1.401(5) .
C30 C31 1.386(5) .
C30 H30 0.9500 .
C31 C32 1.380(5) .
C31 H31 0.9500 .
C32 C33 1.382(5) .
C32 H32 0.9500 .
C33 C34 1.383(5) .
C33 H33 0.9500 .
C34 H34 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 Pd P1 O1 -3.35(11) . .
C27 Pd P1 O1 176.81(11) . .
P1 Pd P1 O1 -15.89(13) 4_565 .
C1 Pd P1 C10 -118.36(15) . .
C27 Pd P1 C10 61.80(15) . .
P1 Pd P1 C10 -130.90(13) 4_565 .
C1 Pd P1 C7 108.56(13) . .
C27 Pd P1 C7 -71.28(14) . .
P1 Pd P1 C7 96.02(12) 4_565 .
C10 P1 O1 C2 133.63(18) . .
C7 P1 O1 C2 -115.47(18) . .
Pd P1 O1 C2 6.23(18) . .
C27 Pd C1 C2 88.2(4) . .
P1 Pd C1 C2 175.9(3) 4_565 .
P1 Pd C1 C2 0.4(2) . .
C27 Pd C1 C2 -88.2(5) . 4_565
P1 Pd C1 C2 -0.4(2) 4_565 4_565
P1 Pd C1 C2 -175.9(3) . 4_565
C2 C1 C2 C3 -0.6(5) 4_565 .
Pd C1 C2 C3 -177.1(2) . .
C2 C1 C2 O1 -179.93(17) 4_565 .
Pd C1 C2 O1 3.6(4) . .
P1 O1 C2 C1 -6.7(3) . .
P1 O1 C2 C3 173.99(19) . .
C1 C2 C3 C4 0.2(4) . .
O1 C2 C3 C4 179.5(3) . .
C2 C3 C4 C3 0.2(6) . 4_565
O1 P1 C7 C9 -49.8(2) . .
C10 P1 C7 C9 56.8(2) . .
Pd P1 C7 C9 -164.20(16) . .
O1 P1 C7 C8 75.12(19) . .
C10 P1 C7 C8 -178.20(18) . .
Pd P1 C7 C8 -39.2(2) . .
O1 P1 C10 C12 161.64(19) . .
C7 P1 C10 C12 55.2(2) . .
Pd P1 C10 C12 -81.4(2) . .
O1 P1 C10 C11 -75.5(2) . .
C7 P1 C10 C11 178.1(2) . .
Pd P1 C10 C11 41.5(2) . .
C1 Pd C27 C28 0.0(3) . .
P1 Pd C27 C28 -87.75(2) 4_565 .
P1 Pd C27 C28 87.75(2) . .
Pd C27 C28 C29 180.000(2) . .
C27 C28 C29 C34 0.000(2) . .
C27 C28 C29 C30 180.000(2) . .
C34 C29 C30 C31 0.000(2) . .
C28 C29 C30 C31 180.000(2) . .
C29 C30 C31 C32 0.000(3) . .
C30 C31 C32 C33 0.000(3) . .
C31 C32 C33 C34 0.000(3) . .
C32 C33 C34 C29 0.000(3) . .
C30 C29 C34 C33 0.000(2) . .
C28 C29 C34 C33 180.000(2) . .
