#------------------------------------------------------------------------------
#$Date: 2019-11-23 18:57:42 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234540 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/51/7125127.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_7125127
loop_
_publ_author_name
'Schuhknecht, Danny'
'Ritter, Florian'
'Tauchert, Michael E.'
_publ_section_title
;
 Isolation and properties of a palladium PBP pincer complex featuring an
 ambiphilic boryl site.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11823
_journal_page_last               11826
_journal_paper_doi               10.1039/c6cc07079e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C40 H40 B P3 Pd'
_chemical_formula_sum            'C40 H40 B P3 Pd'
_chemical_formula_weight         730.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-27 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.699(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6783(16)
_cell_length_b                   18.823(3)
_cell_length_c                   17.516(3)
_cell_measurement_reflns_used    6275
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.21
_cell_volume                     3488.9(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multi opitcal layer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1574 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.6042.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         10149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0407
_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)+(0.0350P)²+0.6040P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                8011
_reflns_number_total             10149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc07079e2.cif
_cod_data_source_block           a15_a52sad
_cod_original_cell_volume        3489.0(9)
_cod_database_code               7125127
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C45(H45), C55(H55), C61(H61), C65(H65), C12(H12), C64(H64),
 C51(H51), C22(H22), C33(H33), C15(H15), C62(H62), C24(H24), C32(H32), C63(H63),
  C23(H23), C41(H41), C44(H44), C52(H52), C13(H13), C31(H31), C14(H14),
 C53(H53), C43(H43), C1AA(H1AA), C54(H54), C34(H34), C42(H42)
2.b Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C81(H81A,H81B,H81C), C70(H70A,H70B,
 H70C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -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_calc_flag
_atom_site_refinement_flags_posn
Pd1 Pd 0.230249(15) 0.281574(9) 0.377568(10) 0.01123(6) Uani 1 d .
P3 P 0.21799(6) 0.20890(3) 0.48812(4) 0.01519(13) Uani 1 d .
P2 P 0.38190(6) 0.22918(3) 0.31706(4) 0.01191(12) Uani 1 d .
P1 P 0.03235(5) 0.32771(3) 0.34282(4) 0.01245(12) Uani 1 d .
C25 C 0.5739(2) 0.28218(12) 0.23196(14) 0.0147(5) Uani 1 d .
H25 H 0.6120 0.2365 0.2348 0.018 Uiso 1 calc R
C21 C 0.4074(2) 0.36175(12) 0.26518(13) 0.0137(4) Uani 1 d .
C40 C 0.5053(2) 0.17691(12) 0.37477(14) 0.0139(4) Uani 1 d .
C45 C 0.5964(2) 0.21235(13) 0.42531(15) 0.0188(5) Uani 1 d .
H45 H 0.5992 0.2628 0.4245 0.023 Uiso 1 calc R
C20 C 0.4653(2) 0.29473(11) 0.26642(13) 0.0124(4) Uani 1 d .
C10 C 0.0374(2) 0.39411(12) 0.26826(14) 0.0143(4) Uani 1 d .
C55 C -0.1112(2) 0.20299(12) 0.33586(15) 0.0165(5) Uani 1 d .
H55 H -0.1015 0.2067 0.3904 0.020 Uiso 1 calc R
C50 C -0.0609(2) 0.25597(12) 0.29277(14) 0.0137(4) Uani 1 d .
C30 C 0.3164(2) 0.16389(12) 0.24512(13) 0.0142(4) Uani 1 d .
C61 C -0.2075(2) 0.36210(12) 0.38582(14) 0.0157(5) Uani 1 d .
H61 H -0.2428 0.3396 0.3393 0.019 Uiso 1 calc R
C65 C -0.0267(2) 0.39643(12) 0.47466(14) 0.0149(5) Uani 1 d .
H65 H 0.0622 0.3976 0.4895 0.018 Uiso 1 calc R
C11 C 0.1592(2) 0.40422(11) 0.24766(13) 0.0133(4) Uani 1 d .
C12 C 0.1642(2) 0.44486(12) 0.18062(14) 0.0172(5) Uani 1 d .
H12 H 0.2435 0.4514 0.1626 0.021 Uiso 1 calc R
C64 C -0.1067(2) 0.42743(12) 0.52196(14) 0.0171(5) Uani 1 d .
H64 H -0.0720 0.4501 0.5685 0.020 Uiso 1 calc R
C60 C -0.0761(2) 0.36379(12) 0.40583(13) 0.0134(4) Uani 1 d .
C51 C -0.0761(2) 0.24921(13) 0.21274(14) 0.0165(5) Uani 1 d .
H51 H -0.0429 0.2846 0.1824 0.020 Uiso 1 calc R
C80 C 0.1046(3) 0.22884(15) 0.55432(16) 0.0263(6) Uani 1 d .
H80A H 0.1243 0.2753 0.5783 0.039 Uiso 1 calc GR
H80B H 0.1096 0.1922 0.5944 0.039 Uiso 1 calc GR
H80C H 0.0191 0.2298 0.5259 0.039 Uiso 1 calc GR
C22 C 0.4680(2) 0.41687(12) 0.23025(14) 0.0164(5) Uani 1 d .
H22 H 0.4356 0.4638 0.2316 0.020 Uiso 1 calc R
C33 C 0.2114(2) 0.05958(13) 0.14242(15) 0.0212(5) Uani 1 d .
H33 H 0.1759 0.0241 0.1075 0.025 Uiso 1 calc R
C15 C -0.0702(2) 0.42693(12) 0.22892(15) 0.0184(5) Uani 1 d .
H15 H -0.1500 0.4211 0.2464 0.022 Uiso 1 calc R
C62 C -0.2866(2) 0.39291(12) 0.43323(15) 0.0176(5) Uani 1 d .
H62 H -0.3756 0.3917 0.4188 0.021 Uiso 1 calc R
C24 C 0.6257(2) 0.33702(13) 0.19364(14) 0.0163(5) Uani 1 d .
H24 H 0.6964 0.3284 0.1673 0.020 Uiso 1 calc R
C32 C 0.1414(2) 0.08793(13) 0.19582(15) 0.0198(5) Uani 1 d .
H32 H 0.0576 0.0718 0.1978 0.024 Uiso 1 calc R
C63 C -0.2365(2) 0.42529(12) 0.50127(14) 0.0174(5) Uani 1 d .
H63 H -0.2909 0.4460 0.5338 0.021 Uiso 1 calc R
C23 C 0.5737(2) 0.40479(13) 0.19389(14) 0.0180(5) Uani 1 d .
H23 H 0.6107 0.4428 0.1691 0.022 Uiso 1 calc R
C41 C 0.5034(2) 0.10276(13) 0.37766(15) 0.0198(5) Uani 1 d .
H41 H 0.4429 0.0772 0.3435 0.024 Uiso 1 calc R
C44 C 0.6831(2) 0.17552(15) 0.47669(15) 0.0242(6) Uani 1 d .
H44 H 0.7453 0.2007 0.5100 0.029 Uiso 1 calc R
C52 C -0.1392(2) 0.19131(13) 0.17698(15) 0.0205(5) Uani 1 d .
H52 H -0.1491 0.1875 0.1224 0.025 Uiso 1 calc R
C13 C 0.0578(2) 0.47576(12) 0.13988(15) 0.0184(5) Uani 1 d .
H13 H 0.0652 0.5026 0.0947 0.022 Uiso 1 calc R
C31 C 0.1936(2) 0.14017(12) 0.24681(14) 0.0166(5) Uani 1 d .
H31 H 0.1447 0.1598 0.2831 0.020 Uiso 1 calc R
C14 C -0.0595(2) 0.46779(12) 0.16457(15) 0.0195(5) Uani 1 d .
H14 H -0.1319 0.4902 0.1375 0.023 Uiso 1 calc R
C53 C -0.1881(2) 0.13882(13) 0.22029(16) 0.0211(5) Uani 1 d .
H53 H -0.2303 0.0989 0.1956 0.025 Uiso 1 calc R
C82 C 0.1828(3) 0.11559(13) 0.46560(16) 0.0258(6) Uani 1 d .
H82A H 0.0987 0.1118 0.4357 0.039 Uiso 1 calc GR
H82B H 0.1848 0.0886 0.5136 0.039 Uiso 1 calc GR
H82C H 0.2460 0.0964 0.4355 0.039 Uiso 1 calc GR
C43 C 0.6789(3) 0.10193(15) 0.47954(16) 0.0277(6) Uani 1 d .
H43 H 0.7372 0.0765 0.5153 0.033 Uiso 1 calc R
C1AA C 0.3865(3) 0.13456(14) 0.19087(16) 0.0248(6) Uani 1 d .
H1AA H 0.4707 0.1501 0.1891 0.030 Uiso 1 calc R
C81 C 0.3623(3) 0.20135(16) 0.55548(16) 0.0284(6) Uani 1 d .
H81A H 0.4285 0.1797 0.5295 0.043 Uiso 1 calc GR
H81B H 0.3467 0.1716 0.5991 0.043 Uiso 1 calc GR
H81C H 0.3895 0.2487 0.5741 0.043 Uiso 1 calc GR
C54 C -0.1749(2) 0.14521(12) 0.30008(16) 0.0198(5) Uani 1 d .
H54 H -0.2096 0.1100 0.3301 0.024 Uiso 1 calc R
C34 C 0.3346(3) 0.08333(15) 0.13995(16) 0.0276(6) Uani 1 d .
H34 H 0.3828 0.0641 0.1031 0.033 Uiso 1 calc R
C42 C 0.5893(3) 0.06593(14) 0.42989(16) 0.0264(6) Uani 1 d .
H42 H 0.5862 0.0155 0.4315 0.032 Uiso 1 calc R
B1 B 0.2810(2) 0.37487(13) 0.30477(16) 0.0136(5) Uani 1 d .
C70 C 0.3101(2) 0.42419(12) 0.38114(15) 0.0191(5) Uani 1 d .
H70A H 0.2302 0.4382 0.3986 0.029 Uiso 1 calc GR
H70B H 0.3563 0.4668 0.3689 0.029 Uiso 1 calc GR
H70C H 0.3612 0.3974 0.4220 0.029 Uiso 1 calc GR
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'
B B 0.0013 0.0007 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P2 Pd1 P3 104.43(2)
P2 Pd1 P1 136.83(2)
P2 Pd1 B1 80.55(7)
P1 Pd1 P3 106.48(2)
B1 Pd1 P3 159.76(7)
B1 Pd1 P1 80.75(7)
C80 P3 Pd1 120.70(9)
C80 P3 C82 101.54(13)
C82 P3 Pd1 114.03(9)
C81 P3 Pd1 115.94(10)
C81 P3 C80 100.42(14)
C81 P3 C82 101.36(14)
C40 P2 Pd1 118.61(8)
C20 P2 Pd1 110.99(7)
C20 P2 C40 105.66(10)
C20 P2 C30 106.64(11)
C30 P2 Pd1 112.44(8)
C30 P2 C40 101.47(11)
C10 P1 Pd1 109.70(8)
C10 P1 C50 103.32(11)
C10 P1 C60 105.09(10)
C50 P1 Pd1 105.71(7)
C50 P1 C60 102.40(10)
C60 P1 Pd1 127.95(8)
C24 C25 C20 119.4(2)
C20 C21 C22 116.3(2)
C20 C21 B1 121.4(2)
C22 C21 B1 122.2(2)
C45 C40 P2 118.79(18)
C45 C40 C41 117.8(2)
C41 C40 P2 122.90(19)
C44 C45 C40 121.4(2)
C25 C20 P2 125.76(17)
C25 C20 C21 122.3(2)
C21 C20 P2 111.96(17)
C11 C10 P1 113.28(17)
C15 C10 P1 123.79(18)
C15 C10 C11 122.6(2)
C54 C55 C50 121.0(2)
C55 C50 P1 119.37(19)
C51 C50 P1 122.10(18)
C51 C50 C55 118.4(2)
C31 C30 P2 118.39(18)
C31 C30 C1AA 118.7(2)
C1AA C30 P2 122.86(19)
C62 C61 C60 120.7(2)
C60 C65 C64 120.5(2)
C10 C11 B1 119.1(2)
C12 C11 C10 115.2(2)
C12 C11 B1 125.5(2)
C13 C12 C11 122.5(2)
C63 C64 C65 120.2(2)
C61 C60 P1 122.23(18)
C65 C60 P1 119.20(17)
C65 C60 C61 118.5(2)
C52 C51 C50 120.7(2)
C23 C22 C21 121.9(2)
C32 C33 C34 119.7(2)
C14 C15 C10 119.6(2)
C63 C62 C61 120.3(2)
C25 C24 C23 119.7(2)
C33 C32 C31 120.1(2)
C62 C63 C64 119.8(2)
C22 C23 C24 120.1(2)
C42 C41 C40 120.7(2)
C45 C44 C43 120.1(3)
C51 C52 C53 120.5(2)
C12 C13 C14 120.4(2)
C30 C31 C32 120.7(2)
C15 C14 C13 119.4(2)
C52 C53 C54 119.5(2)
C42 C43 C44 119.3(2)
C34 C1AA C30 120.7(2)
C55 C54 C53 119.9(2)
C1AA C34 C33 120.2(2)
C43 C42 C41 120.6(2)
C21 B1 Pd1 113.40(15)
C21 B1 C11 115.6(2)
C21 B1 C70 111.24(19)
C11 B1 Pd1 112.04(15)
C70 B1 Pd1 90.76(15)
C70 B1 C11 111.17(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 P3 2.3888(7)
Pd1 P2 2.2756(6)
Pd1 P1 2.2904(7)
Pd1 B1 2.278(3)
P3 C80 1.824(3)
P3 C82 1.828(3)
P3 C81 1.817(3)
P2 C40 1.835(2)
P2 C20 1.820(2)
P2 C30 1.830(2)
P1 C10 1.814(2)
P1 C50 1.830(2)
P1 C60 1.834(2)
C25 C20 1.398(3)
C25 C24 1.386(3)
C21 C20 1.403(3)
C21 C22 1.405(3)
C21 B1 1.617(3)
C40 C45 1.395(3)
C40 C41 1.397(3)
C45 C44 1.387(4)
C10 C11 1.409(3)
C10 C15 1.402(3)
C55 C50 1.401(3)
C55 C54 1.387(3)
C50 C51 1.395(3)
C30 C31 1.389(3)
C30 C1AA 1.399(3)
C61 C60 1.400(3)
C61 C62 1.389(3)
C65 C64 1.395(3)
C65 C60 1.392(3)
C11 C12 1.408(3)
C11 B1 1.627(4)
C12 C13 1.386(3)
C64 C63 1.386(3)
C51 C52 1.386(3)
C22 C23 1.387(3)
C33 C32 1.380(4)
C33 C34 1.395(4)
C15 C14 1.382(3)
C62 C63 1.381(3)
C24 C23 1.391(3)
C32 C31 1.394(3)
C41 C42 1.390(3)
C44 C43 1.387(4)
C52 C53 1.389(4)
C13 C14 1.387(3)
C53 C54 1.391(4)
C43 C42 1.382(4)
C1AA C34 1.379(4)
B1 C70 1.624(4)
