#------------------------------------------------------------------------------
#$Date: 2021-11-17 02:12:00 +0200 (Wed, 17 Nov 2021) $
#$Revision: 270706 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708855.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_7708855
loop_
_publ_author_name
'Cabeza, Javier A.'
'Fernández, Israel'
'García-Álvarez, Pablo'
'García-Soriano, Rubén'
'Laglera-Gándara, Carlos J'
'Toral, Rubén'
_publ_section_title
;
 Stannylenes based on pyrrole-phosphane and dipyrromethane-diphosphane
 scaffolds: syntheses and behavior as precursors to PSnP pincer
 palladium(II), palladium(0) and gold(I) complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16122
_journal_page_last               16132
_journal_paper_doi               10.1039/d1dt02967c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C25 H42 Cl2 N2 P2 Pd Sn, 0.5(C6 D6)'
_chemical_formula_sum            'C28 H42 Cl2 D3 N2 P2 Pd Sn'
_chemical_formula_weight         770.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2021-10-05 deposited with the CCDC.	2021-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.654(3)
_cell_angle_beta                 108.540(3)
_cell_angle_gamma                103.841(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7876(4)
_cell_length_b                   12.4560(5)
_cell_length_c                   13.6800(3)
_cell_measurement_reflns_used    10423
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.4890
_cell_measurement_theta_min      3.5620
_cell_volume                     1613.14(11)
_computing_cell_refinement
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2018)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15094
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.628
_diffrn_reflns_theta_min         3.575
_exptl_absorpt_coefficient_mu    13.258
_exptl_absorpt_correction_T_max  0.402
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.281
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.519
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+0.4877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5558
_reflns_number_total             5965
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02967c2.cif
_cod_data_source_block           7-21014-rgs34
_cod_original_cell_volume        1613.14(10)
_cod_database_code               7708855
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2842(4) 0.2593(4) 0.6107(3) 0.0472(9) Uani 1 1 d . . . . .
H1A H 0.3607 0.2372 0.6529 0.071 Uiso 1 1 calc R U . . .
H1B H 0.1961 0.2001 0.5943 0.071 Uiso 1 1 calc R U . . .
H1C H 0.2865 0.3341 0.6525 0.071 Uiso 1 1 calc R U . . .
C2 C 0.4275(4) 0.3695(3) 0.5245(3) 0.0419(8) Uani 1 1 d . . . . .
H2A H 0.4145 0.4435 0.5510 0.063 Uiso 1 1 calc R U . . .
H2B H 0.4422 0.3657 0.4570 0.063 Uiso 1 1 calc R U . . .
H2C H 0.5083 0.3632 0.5788 0.063 Uiso 1 1 calc R U . . .
C3 C 0.2990(3) 0.2697(3) 0.5041(3) 0.0343(7) Uani 1 1 d . . . . .
H3 H 0.3112 0.1964 0.4692 0.041 Uiso 1 1 calc R U . . .
C4 C 0.0281(4) 0.0434(3) 0.3642(3) 0.0452(8) Uani 1 1 d . . . . .
H4A H -0.0561 -0.0215 0.3453 0.068 Uiso 1 1 calc R U . . .
H4B H 0.0992 0.0452 0.4309 0.068 Uiso 1 1 calc R U . . .
H4C H 0.0618 0.0338 0.3055 0.068 Uiso 1 1 calc R U . . .
C5 C -0.1293(4) 0.1507(3) 0.2844(3) 0.0437(8) Uani 1 1 d . . . . .
H5A H -0.1093 0.1358 0.2188 0.066 Uiso 1 1 calc R U . . .
H5B H -0.1485 0.2242 0.2967 0.066 Uiso 1 1 calc R U . . .
H5C H -0.2102 0.0875 0.2755 0.066 Uiso 1 1 calc R U . . .
C6 C -0.0042(3) 0.1576(3) 0.3815(3) 0.0360(7) Uani 1 1 d . . . . .
H6 H -0.0291 0.1691 0.4464 0.043 Uiso 1 1 calc R U . . .
C7 C 0.1016(3) 0.4013(3) 0.4846(2) 0.0319(6) Uani 1 1 d . . . . .
H7A H 0.0013 0.3873 0.4485 0.038 Uiso 1 1 calc R U . . .
H7B H 0.1177 0.3924 0.5575 0.038 Uiso 1 1 calc R U . . .
C8 C 0.1764(3) 0.5249(3) 0.4989(2) 0.0297(6) Uani 1 1 d . . . . .
C9 C 0.2695(3) 0.6131(3) 0.5884(2) 0.0352(7) Uani 1 1 d . . . . .
H9 H 0.3054 0.6081 0.6597 0.042 Uiso 1 1 calc R U . . .
C10 C 0.3027(3) 0.7133(3) 0.5555(3) 0.0362(7) Uani 1 1 d . . . . .
H10 H 0.3653 0.7877 0.6010 0.043 Uiso 1 1 calc R U . . .
C11 C 0.2288(3) 0.6843(3) 0.4468(2) 0.0324(6) Uani 1 1 d . . . . .
C12 C 0.2210(4) 0.7570(3) 0.3692(3) 0.0359(7) Uani 1 1 d . . . . .
C13 C 0.0752(4) 0.7685(3) 0.3292(3) 0.0401(7) Uani 1 1 d . . . . .
H13A H 0.0064 0.6917 0.2875 0.060 Uiso 1 1 calc R U . . .
H13B H 0.0715 0.8196 0.2832 0.060 Uiso 1 1 calc R U . . .
H13C H 0.0551 0.8014 0.3915 0.060 Uiso 1 1 calc R U . . .
C14 C 0.3267(5) 0.8776(3) 0.4286(3) 0.0498(9) Uani 1 1 d . . . . .
H14A H 0.3091 0.9129 0.4915 0.075 Uiso 1 1 calc R U . . .
H14B H 0.3189 0.9257 0.3799 0.075 Uiso 1 1 calc R U . . .
H14C H 0.4200 0.8718 0.4527 0.075 Uiso 1 1 calc R U . . .
C15 C 0.2476(3) 0.7023(3) 0.2712(2) 0.0313(6) Uani 1 1 d . . . . .
C16 C 0.3359(3) 0.7467(3) 0.2260(3) 0.0374(7) Uani 1 1 d . . . . .
H16 H 0.4012 0.8227 0.2529 0.045 Uiso 1 1 calc R U . . .
C17 C 0.3134(3) 0.6596(3) 0.1317(3) 0.0374(7) Uani 1 1 d . . . . .
H17 H 0.3605 0.6668 0.0841 0.045 Uiso 1 1 calc R U . . .
C18 C 0.2114(3) 0.5632(3) 0.1216(2) 0.0306(6) Uani 1 1 d . . . . .
C19 C 0.1472(3) 0.4458(3) 0.0408(2) 0.0318(6) Uani 1 1 d . . . . .
H19A H 0.1739 0.4500 -0.0216 0.038 Uiso 1 1 calc R U . . .
H19B H 0.0456 0.4274 0.0143 0.038 Uiso 1 1 calc R U . . .
C20 C 0.3629(3) 0.3340(3) 0.0869(3) 0.0380(7) Uani 1 1 d . . . . .
H20 H 0.3799 0.2606 0.0964 0.046 Uiso 1 1 calc R U . . .
C21 C 0.4717(4) 0.4330(4) 0.1844(3) 0.0509(9) Uani 1 1 d . . . . .
H21A H 0.5639 0.4377 0.1849 0.076 Uiso 1 1 calc R U . . .
H21B H 0.4660 0.4189 0.2509 0.076 Uiso 1 1 calc R U . . .
H21C H 0.4552 0.5063 0.1798 0.076 Uiso 1 1 calc R U . . .
C22 C 0.3780(5) 0.3457(4) -0.0184(4) 0.0565(10) Uani 1 1 d . . . . .
H22A H 0.3684 0.4196 -0.0278 0.085 Uiso 1 1 calc R U . . .
H22B H 0.3060 0.2816 -0.0796 0.085 Uiso 1 1 calc R U . . .
H22C H 0.4693 0.3433 -0.0153 0.085 Uiso 1 1 calc R U . . .
C23 C 0.0681(4) 0.2007(3) -0.0357(3) 0.0388(7) Uani 1 1 d . . . . .
H23 H 0.0660 0.2261 -0.1008 0.047 Uiso 1 1 calc R U . . .
C24 C -0.0777(4) 0.1736(3) -0.0356(3) 0.0506(9) Uani 1 1 d . . . . .
H24A H -0.1419 0.1093 -0.1002 0.076 Uiso 1 1 calc R U . . .
H24B H -0.1067 0.2424 -0.0359 0.076 Uiso 1 1 calc R U . . .
H24C H -0.0780 0.1518 0.0293 0.076 Uiso 1 1 calc R U . . .
C25 C 0.1132(4) 0.0928(3) -0.0450(3) 0.0457(8) Uani 1 1 d . . . . .
H25A H 0.1287 0.0722 0.0223 0.069 Uiso 1 1 calc R U . . .
H25B H 0.1991 0.1090 -0.0580 0.069 Uiso 1 1 calc R U . . .
H25C H 0.0407 0.0282 -0.1054 0.069 Uiso 1 1 calc R U . . .
C26 C -0.4667(5) 0.0946(5) 0.0842(5) 0.0744(17) Uani 1 1 d . . . . .
C27 C -0.4078(6) 0.1001(5) 0.0097(6) 0.0787(17) Uani 1 1 d . . . . .
C28 C -0.4414(6) 0.0056(6) -0.0739(5) 0.0731(15) Uani 1 1 d . . . . .
Cl1 Cl -0.15914(7) 0.43592(7) 0.18415(6) 0.03792(17) Uani 1 1 d . . . . .
Cl2 Cl 0.28114(9) 0.15393(7) 0.24585(6) 0.04060(19) Uani 1 1 d . . . . .
N1 N 0.1476(3) 0.5684(2) 0.4119(2) 0.0293(5) Uani 1 1 d . . . . .
N2 N 0.1681(3) 0.5894(2) 0.2060(2) 0.0296(5) Uani 1 1 d . . . . .
P1 P 0.14504(8) 0.28427(6) 0.40733(6) 0.02780(16) Uani 1 1 d . . . . .
P2 P 0.18903(8) 0.32217(6) 0.08447(6) 0.02721(16) Uani 1 1 d . . . . .
Pd1 Pd 0.17075(2) 0.29626(2) 0.24541(2) 0.02674(8) Uani 1 1 d . . . . .
Sn1 Sn 0.07914(2) 0.45922(2) 0.25782(2) 0.02543(8) Uani 1 1 d . . . . .
D26 D -0.452(4) 0.145(4) 0.130(3) 0.031 Uiso 1 1 d . U . . .
D27 D -0.358(4) 0.157(4) 0.014(3) 0.031 Uiso 1 1 d . U . . .
D28 D -0.398(4) 0.016(3) -0.119(3) 0.031 Uiso 1 1 d . U . . .
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
Sn Sn 0.0259 5.4591 '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
_geom_angle_publ_flag
C2 C3 C1 111.7(3) . . ?
C2 C3 P1 110.0(2) . . ?
C1 C3 P1 113.2(2) . . ?
C4 C6 C5 110.6(3) . . ?
C4 C6 P1 112.7(2) . . ?
C5 C6 P1 110.2(2) . . ?
C8 C7 P1 118.6(2) . . ?
C9 C8 N1 108.3(3) . . ?
C9 C8 C7 131.6(3) . . ?
N1 C8 C7 120.0(3) . . ?
C8 C9 C10 107.5(3) . . ?
C11 C10 C9 108.0(3) . . ?
C10 C11 N1 107.6(3) . . ?
C10 C11 C12 131.1(3) . . ?
N1 C11 C12 121.2(3) . . ?
C14 C12 C11 109.3(3) . . ?
C14 C12 C15 109.5(3) . . ?
C11 C12 C15 111.9(2) . . ?
C14 C12 C13 108.6(3) . . ?
C11 C12 C13 109.1(3) . . ?
C15 C12 C13 108.3(3) . . ?
C16 C15 N2 107.9(3) . . ?
C16 C15 C12 131.4(3) . . ?
N2 C15 C12 120.6(3) . . ?
C15 C16 C17 108.0(3) . . ?
C18 C17 C16 107.6(3) . . ?
C17 C18 N2 108.0(3) . . ?
C17 C18 C19 131.9(3) . . ?
N2 C18 C19 120.1(3) . . ?
C18 C19 P2 118.1(2) . . ?
C21 C20 C22 111.3(3) . . ?
C21 C20 P2 110.5(2) . . ?
C22 C20 P2 113.2(3) . . ?
C24 C23 C25 111.4(3) . . ?
C24 C23 P2 109.8(2) . . ?
C25 C23 P2 112.6(2) . . ?
C28 C26 C27 119.8(5) 2_455 . ?
C28 C27 C26 120.2(5) . . ?
C26 C28 C27 120.0(5) 2_455 . ?
C8 N1 C11 108.5(3) . . ?
C8 N1 Sn1 119.80(19) . . ?
C11 N1 Sn1 124.9(2) . . ?
C15 N2 C18 108.4(3) . . ?
C15 N2 Sn1 125.2(2) . . ?
C18 N2 Sn1 119.99(19) . . ?
C3 P1 C6 107.59(15) . . ?
C3 P1 C7 106.14(15) . . ?
C6 P1 C7 100.13(15) . . ?
C3 P1 Pd1 111.93(10) . . ?
C6 P1 Pd1 110.75(11) . . ?
C7 P1 Pd1 119.22(10) . . ?
C20 P2 C23 106.32(16) . . ?
C20 P2 C19 106.05(15) . . ?
C23 P2 C19 100.06(15) . . ?
C20 P2 Pd1 111.30(11) . . ?
C23 P2 Pd1 112.72(11) . . ?
C19 P2 Pd1 119.16(10) . . ?
P1 Pd1 P2 174.94(2) . . ?
P1 Pd1 Cl2 91.78(3) . . ?
P2 Pd1 Cl2 93.25(3) . . ?
P1 Pd1 Sn1 87.475(18) . . ?
P2 Pd1 Sn1 87.464(18) . . ?
Cl2 Pd1 Sn1 174.07(2) . . ?
N1 Sn1 N2 92.05(10) . . ?
N1 Sn1 Cl1 103.96(7) . . ?
N2 Sn1 Cl1 103.62(7) . . ?
N1 Sn1 Pd1 114.14(7) . . ?
N2 Sn1 Pd1 114.61(7) . . ?
Cl1 Sn1 Pd1 123.45(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.544(5) . ?
C2 C3 1.528(5) . ?
C3 P1 1.840(3) . ?
C4 C6 1.534(5) . ?
C5 C6 1.533(5) . ?
C6 P1 1.845(3) . ?
C7 C8 1.498(5) . ?
C7 P1 1.865(3) . ?
C8 C9 1.364(5) . ?
C8 N1 1.384(4) . ?
C9 C10 1.416(5) . ?
C10 C11 1.367(4) . ?
C11 N1 1.389(4) . ?
C11 C12 1.524(4) . ?
C12 C14 1.521(5) . ?
C12 C15 1.521(4) . ?
C12 C13 1.545(5) . ?
C15 C16 1.362(5) . ?
C15 N2 1.393(4) . ?
C16 C17 1.417(5) . ?
C17 C18 1.369(5) . ?
C18 N2 1.386(4) . ?
C18 C19 1.488(4) . ?
C19 P2 1.861(3) . ?
C20 C21 1.524(5) . ?
C20 C22 1.532(5) . ?
C20 P2 1.834(3) . ?
C23 C24 1.528(5) . ?
C23 C25 1.530(5) . ?
C23 P2 1.839(3) . ?
C26 C28 1.345(9) 2_455 ?
C26 C27 1.366(9) . ?
C27 C28 1.346(9) . ?
C28 C26 1.345(9) 2_455 ?
Cl1 Sn1 2.3632(7) . ?
Cl2 Pd1 2.3604(7) . ?
N1 Sn1 2.051(2) . ?
N2 Sn1 2.051(3) . ?
P1 Pd1 2.3475(7) . ?
P2 Pd1 2.3500(7) . ?
Pd1 Sn1 2.4602(3) . ?
