#------------------------------------------------------------------------------
#$Date: 2021-01-07 05:46:17 +0100 (jue 07 de ene de 2021) $
#$Revision: 260659 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/74/7127422.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_7127422
loop_
_publ_author_name
'Cabeza, Javier A.'
'García-Álvarez, Pablo'
'Laglera-Gándara, Carlos J'
'Pérez-Carreño, Enrique'
_publ_section_title
;
 A Z-type PGeP pincer germylene ligand in a T-shaped palladium(0) complex.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14095
_journal_page_last               14097
_journal_paper_doi               10.1039/d0cc06614a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C25 H42 Cl2 Ge N2 P2 Pd'
_chemical_formula_sum            'C25 H42 Cl2 Ge N2 P2 Pd'
_chemical_formula_weight         682.43
_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
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2020-10-02 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.665(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4960(2)
_cell_length_b                   18.4130(3)
_cell_length_c                   14.6710(3)
_cell_measurement_reflns_used    11320
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      69.4910
_cell_measurement_theta_min      3.9980
_cell_volume                     2975.06(10)
_computing_cell_refinement
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_data_collection
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)'
_computing_molecular_graphics
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2020)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         69.641
_diffrn_reflns_theta_min         3.957
_exptl_absorpt_coefficient_mu    8.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0612P)²+1.1646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5074
_reflns_number_total             5525
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc06614a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7127422--7127423.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7127422
_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+1/2, -z+1/2'
'-x, -y, -z'
'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_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 0.3854(5) 0.2668(3) 0.1671(6) 0.109(2) Uani 1 1 d . . . . .
H1A H 0.3108 0.2954 0.1440 0.163 Uiso 1 1 calc R U . . .
H1B H 0.4112 0.2495 0.1128 0.163 Uiso 1 1 calc R U . . .
H1C H 0.4493 0.2972 0.2079 0.163 Uiso 1 1 calc R U . . .
C2 C 0.3643(6) 0.2243(4) 0.3223(5) 0.114(2) Uani 1 1 d . . . . .
H2A H 0.4427 0.2470 0.3539 0.170 Uiso 1 1 calc R U . . .
H2B H 0.3532 0.1814 0.3584 0.170 Uiso 1 1 calc R U . . .
H2C H 0.2988 0.2591 0.3194 0.170 Uiso 1 1 calc R U . . .
C3 C 0.3617(4) 0.2023(2) 0.2239(4) 0.0677(13) Uani 1 1 d . . . . .
H3 H 0.4311 0.1680 0.2305 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1373(5) 0.0524(2) 0.0239(3) 0.0592(10) Uani 1 1 d . . . . .
H4A H 0.0559 0.0729 0.0138 0.089 Uiso 1 1 calc R U . . .
H4B H 0.1517 0.0151 0.0735 0.089 Uiso 1 1 calc R U . . .
H4C H 0.1436 0.0307 -0.0354 0.089 Uiso 1 1 calc R U . . .
C5 C 0.2261(8) 0.1653(3) -0.0221(5) 0.109(2) Uani 1 1 d . . . . .
H5A H 0.2333 0.1396 -0.0787 0.163 Uiso 1 1 calc R U . . .
H5B H 0.2928 0.2002 -0.0011 0.163 Uiso 1 1 calc R U . . .
H5C H 0.1484 0.1912 -0.0375 0.163 Uiso 1 1 calc R U . . .
C6 C 0.2316(4) 0.1124(2) 0.0548(3) 0.0641(11) Uani 1 1 d . . . . .
H6 H 0.3127 0.0883 0.0686 0.077 Uiso 1 1 calc R U . . .
C7 C 0.0988(3) 0.21884(18) 0.1428(3) 0.0456(8) Uani 1 1 d . . . . .
H7A H 0.1053 0.2472 0.2014 0.055 Uiso 1 1 calc R U . . .
H7B H 0.1117 0.2529 0.0943 0.055 Uiso 1 1 calc R U . . .
C8 C -0.0269(3) 0.18875(18) 0.1078(3) 0.0433(7) Uani 1 1 d . . . . .
C9 C -0.1139(3) 0.1979(2) 0.0236(3) 0.0490(8) Uani 1 1 d . . . . .
H9 H -0.1068 0.2265 -0.0284 0.059 Uiso 1 1 calc R U . . .
C10 C -0.2175(3) 0.1570(2) 0.0271(3) 0.0495(8) Uani 1 1 d . . . . .
H10 H -0.2916 0.1531 -0.0224 0.059 Uiso 1 1 calc R U . . .
C11 C -0.1914(3) 0.12414(18) 0.1146(2) 0.0397(7) Uani 1 1 d . . . . .
C12 C -0.2734(3) 0.08241(18) 0.1600(2) 0.0400(7) Uani 1 1 d . . . . .
C13 C -0.3229(3) 0.13576(19) 0.2207(3) 0.0479(8) Uani 1 1 d . . . . .
H13A H -0.2553 0.1557 0.2713 0.072 Uiso 1 1 calc R U . . .
H13B H -0.3788 0.1101 0.2490 0.072 Uiso 1 1 calc R U . . .
H13C H -0.3662 0.1754 0.1804 0.072 Uiso 1 1 calc R U . . .
C14 C -0.3816(3) 0.0510(2) 0.0828(3) 0.0560(10) Uani 1 1 d . . . . .
H14A H -0.4272 0.0906 0.0440 0.084 Uiso 1 1 calc R U . . .
H14B H -0.4348 0.0245 0.1129 0.084 Uiso 1 1 calc R U . . .
H14C H -0.3519 0.0177 0.0423 0.084 Uiso 1 1 calc R U . . .
C15 C -0.2101(2) 0.02142(18) 0.2249(2) 0.0370(7) Uani 1 1 d . . . . .
C16 C -0.2541(3) -0.04172(18) 0.2494(3) 0.0447(8) Uani 1 1 d . . . . .
H16 H -0.3331 -0.0608 0.2214 0.054 Uiso 1 1 calc R U . . .
C17 C -0.1616(3) -0.07452(19) 0.3241(3) 0.0452(7) Uani 1 1 d . . . . .
H17 H -0.1674 -0.1193 0.3547 0.054 Uiso 1 1 calc R U . . .
C18 C -0.0636(3) -0.02989(17) 0.3434(2) 0.0367(6) Uani 1 1 d . . . . .
C19 C 0.0595(3) -0.0384(2) 0.4138(2) 0.0413(7) Uani 1 1 d . . . . .
H19A H 0.0595 -0.0831 0.4513 0.050 Uiso 1 1 calc R U . . .
H19B H 0.0737 0.0032 0.4584 0.050 Uiso 1 1 calc R U . . .
C20 C 0.1644(4) -0.1320(2) 0.3000(3) 0.0587(10) Uani 1 1 d . . . . .
H20 H 0.1344 -0.1669 0.3405 0.070 Uiso 1 1 calc R U . . .
C21 C 0.0673(5) -0.1260(2) 0.2050(3) 0.0665(11) Uani 1 1 d . . . . .
H21A H 0.0980 -0.0966 0.1612 0.100 Uiso 1 1 calc R U . . .
H21B H -0.0052 -0.1028 0.2144 0.100 Uiso 1 1 calc R U . . .
H21C H 0.0463 -0.1746 0.1782 0.100 Uiso 1 1 calc R U . . .
C22 C 0.2814(6) -0.1628(3) 0.2867(5) 0.098(2) Uani 1 1 d . . . . .
H22A H 0.2637 -0.2081 0.2504 0.147 Uiso 1 1 calc R U . . .
H22B H 0.3390 -0.1724 0.3491 0.147 Uiso 1 1 calc R U . . .
H22C H 0.3167 -0.1276 0.2521 0.147 Uiso 1 1 calc R U . . .
C23 C 0.3205(3) -0.0493(3) 0.4652(3) 0.0768(16) Uani 1 1 d . . . . .
H23 H 0.3913 -0.0615 0.4413 0.092 Uiso 1 1 calc R U . . .
C24 C 0.3460(4) 0.0253(5) 0.5123(4) 0.105(2) Uani 1 1 d . . . . .
H24A H 0.2756 0.0411 0.5322 0.158 Uiso 1 1 calc R U . . .
H24B H 0.3614 0.0604 0.4669 0.158 Uiso 1 1 calc R U . . .
H24C H 0.4174 0.0223 0.5681 0.158 Uiso 1 1 calc R U . . .
C25 C 0.3099(5) -0.1101(5) 0.5334(4) 0.130(3) Uani 1 1 d . . . . .
H25A H 0.3866 -0.1145 0.5840 0.194 Uiso 1 1 calc R U . . .
H25B H 0.2920 -0.1560 0.4985 0.194 Uiso 1 1 calc R U . . .
H25C H 0.2443 -0.0987 0.5615 0.194 Uiso 1 1 calc R U . . .
Cl1 Cl 0.03562(7) 0.17078(5) 0.39112(6) 0.0486(2) Uani 1 1 d . . . . .
Cl2 Cl 0.40093(7) 0.01240(5) 0.25694(6) 0.0500(2) Uani 1 1 d . . . . .
Ge1 Ge 0.02298(3) 0.09607(2) 0.27103(2) 0.03281(11) Uani 1 1 d . . . . .
N1 N -0.0740(2) 0.14394(15) 0.16554(19) 0.0386(6) Uani 1 1 d . . . . .
N2 N -0.0918(2) 0.02945(14) 0.28385(18) 0.0351(5) Uani 1 1 d . . . . .
P1 P 0.22188(7) 0.15011(5) 0.16886(7) 0.0434(2) Uani 1 1 d . . . . .
P2 P 0.18667(7) -0.04358(5) 0.36072(6) 0.0408(2) Uani 1 1 d . . . . .
Pd1 Pd 0.20884(2) 0.05314(2) 0.26577(2) 0.03576(10) Uani 1 1 d . . . . .
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'
Ge Ge -1.0885 0.8855 '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'
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 111.1(5) . . ?
C2 C3 P1 109.7(3) . . ?
C1 C3 P1 115.9(4) . . ?
C5 C6 C4 112.3(5) . . ?
C5 C6 P1 116.4(4) . . ?
C4 C6 P1 108.7(3) . . ?
C8 C7 P1 115.0(2) . . ?
C9 C8 N1 108.2(3) . . ?
C9 C8 C7 130.8(3) . . ?
N1 C8 C7 121.0(3) . . ?
C8 C9 C10 107.9(3) . . ?
C11 C10 C9 107.8(3) . . ?
C10 C11 N1 107.8(3) . . ?
C10 C11 C12 129.8(3) . . ?
N1 C11 C12 121.9(3) . . ?
C11 C12 C15 113.9(2) . . ?
C11 C12 C14 110.0(3) . . ?
C15 C12 C14 109.0(3) . . ?
C11 C12 C13 108.1(3) . . ?
C15 C12 C13 107.4(3) . . ?
C14 C12 C13 108.1(3) . . ?
C16 C15 N2 107.4(3) . . ?
C16 C15 C12 130.7(3) . . ?
N2 C15 C12 121.2(3) . . ?
C15 C16 C17 108.3(3) . . ?
C18 C17 C16 107.2(3) . . ?
C17 C18 N2 108.5(3) . . ?
C17 C18 C19 130.0(3) . . ?
N2 C18 C19 121.5(3) . . ?
C18 C19 P2 114.8(2) . . ?
C21 C20 C22 110.7(4) . . ?
C21 C20 P2 110.1(3) . . ?
C22 C20 P2 112.7(4) . . ?
C24 C23 C25 113.8(5) . . ?
C24 C23 P2 109.4(4) . . ?
C25 C23 P2 112.5(4) . . ?
N2 Ge1 N1 97.16(11) . . ?
N2 Ge1 Cl1 102.57(8) . . ?
N1 Ge1 Cl1 104.88(9) . . ?
N2 Ge1 Pd1 118.18(8) . . ?
N1 Ge1 Pd1 118.56(8) . . ?
Cl1 Ge1 Pd1 113.07(3) . . ?
C11 N1 C8 108.3(3) . . ?
C11 N1 Ge1 125.7(2) . . ?
C8 N1 Ge1 122.9(2) . . ?
C18 N2 C15 108.6(3) . . ?
C18 N2 Ge1 123.0(2) . . ?
C15 N2 Ge1 127.2(2) . . ?
C6 P1 C3 108.7(2) . . ?
C6 P1 C7 108.1(2) . . ?
C3 P1 C7 104.61(17) . . ?
C6 P1 Pd1 107.37(14) . . ?
C3 P1 Pd1 109.52(18) . . ?
C7 P1 Pd1 118.26(11) . . ?
C23 P2 C20 108.7(2) . . ?
C23 P2 C19 103.08(17) . . ?
C20 P2 C19 103.46(18) . . ?
C23 P2 Pd1 109.56(17) . . ?
C20 P2 Pd1 114.41(13) . . ?
C19 P2 Pd1 116.76(12) . . ?
Ge1 Pd1 P1 88.85(2) . . ?
Ge1 Pd1 P2 88.89(2) . . ?
P1 Pd1 P2 177.51(3) . . ?
Ge1 Pd1 Cl2 178.00(3) . . ?
P1 Pd1 Cl2 89.15(3) . . ?
P2 Pd1 Cl2 93.12(3) . . ?
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 1.520(8) . ?
C2 C3 1.493(8) . ?
C3 P1 1.848(4) . ?
C4 C6 1.522(6) . ?
C5 C6 1.479(7) . ?
C6 P1 1.844(4) . ?
C7 C8 1.495(5) . ?
C7 P1 1.854(3) . ?
C8 C9 1.358(5) . ?
C8 N1 1.398(4) . ?
C9 C10 1.423(5) . ?
C10 C11 1.372(5) . ?
C11 N1 1.391(4) . ?
C11 C12 1.511(4) . ?
C12 C15 1.517(5) . ?
C12 C14 1.535(5) . ?
C12 C13 1.540(5) . ?
C15 C16 1.357(5) . ?
C15 N2 1.394(4) . ?
C16 C17 1.425(5) . ?
C17 C18 1.357(5) . ?
C18 N2 1.378(4) . ?
C18 C19 1.502(4) . ?
C19 P2 1.845(3) . ?
C20 C21 1.519(7) . ?
C20 C22 1.523(6) . ?
C20 P2 1.838(4) . ?
C23 C24 1.528(9) . ?
C23 C25 1.530(8) . ?
C23 P2 1.837(4) . ?
Cl1 Ge1 2.2070(8) . ?
Cl2 Pd1 2.3707(7) . ?
Ge1 N2 1.851(2) . ?
Ge1 N1 1.851(3) . ?
Ge1 Pd1 2.3001(4) . ?
P1 Pd1 2.3138(9) . ?
P2 Pd1 2.3197(9) . ?
