 
data_241029RAL_LLR_PdBr_100KB
 
_audit_creation_method            'SHELXL-2019/1'
_shelx_SHELXL_version_number      '2019/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety    'C36 H61 Br P2 Pd, 2(C H Cl3)' 
_chemical_formula_sum             'C38 H63 Br Cl6 P2 Pd' 
_chemical_formula_weight          980.83

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'
 'Br'  'Br'  -0.6763   1.2805
 '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'
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            62
_space_group_name_H-M_alt         'P n m a'
_space_group_name_Hall            '-P 2ac 2n'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    12.35740(10)
_cell_length_b                    17.36720(10)
_cell_length_c                    19.7634(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      4241.49(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     27861
_cell_measurement_theta_min       3.340
_cell_measurement_theta_max       75.769
 
_exptl_crystal_description        prism
_exptl_crystal_colour             yellow
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.536          
_exptl_crystal_F_000              2016
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.119
_exptl_crystal_size_mid           0.080
_exptl_crystal_size_min           0.072
_exptl_absorpt_coefficient_mu     9.021
_shelx_estimated_absorpt_T_min    0.411
_shelx_estimated_absorpt_T_max    0.571
_exptl_absorpt_correction_T_min                   0.64446
_exptl_absorpt_correction_T_max                   0.66764
_exptl_absorpt_correction_type            multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.141a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min           0.746
_oxdiff_exptl_absorpt_empirical_full_max           1.490
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature       100(2)
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_monochromator mirror
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_type HyPix
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number             38741
_diffrn_reflns_av_unetI/netI      0.0228
_diffrn_reflns_av_R_equivalents   0.0443
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          3.388
_diffrn_reflns_theta_max          75.979
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.962
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.962
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.962
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              4405
_reflns_number_gt                 4174
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_cell_refinement     'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction      'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_structure_solution     'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     'SHELXTL'
_computing_publication_material   'SHELXTL'
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0209P)²+3.4263P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          4405
_refine_ls_number_parameters      232
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0235
_refine_ls_R_factor_gt            0.0220
_refine_ls_wR_factor_ref          0.0554
_refine_ls_wR_factor_gt           0.0546
_refine_ls_goodness_of_fit_ref    1.104
_refine_ls_restrained_S_all       1.104
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
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
Pd1 Pd 0.75747(2) 0.750000 0.44449(2) 0.01027(6) Uani 1 2 d S T P . .
Br1 Br 0.59636(2) 0.750000 0.52568(2) 0.01890(7) Uani 1 2 d S T P . .
P1 P 0.78292(3) 0.61911(3) 0.44195(2) 0.01126(9) Uani 1 1 d . . . . .
Cl2 Cl 0.71646(6) 0.750000 -0.06305(3) 0.02685(15) Uani 1 2 d S T P . .
Cl3 Cl 0.74667(4) 0.66656(3) 0.06225(2) 0.02634(11) Uani 1 1 d . . . . .
Cl1 Cl 0.48574(6) 0.750000 0.72472(4) 0.03339(17) Uani 1 2 d S T P . .
Cl Cl 0.68531(5) 0.83328(3) 0.74883(3) 0.03843(13) Uani 1 1 d . . . . .
C16 C 0.79994(13) 0.67835(10) 0.27946(9) 0.0128(3) Uani 1 1 d . . . . .
H16A H 0.803868 0.631631 0.250856 0.015 Uiso 1 1 calc R U . . .
H16B H 0.729591 0.677912 0.303419 0.015 Uiso 1 1 calc R U . . .
C15 C 0.88699(18) 0.750000 0.37628(12) 0.0111(5) Uani 1 2 d S T P . .
H15 H 0.954378 0.749999 0.404289 0.013 Uiso 1 2 calc R U P . .
C17 C 0.80701(19) 0.750000 0.23464(12) 0.0133(5) Uani 1 2 d S T P . .
H17 H 0.745732 0.750000 0.201595 0.016 Uiso 1 2 calc R U P . .
C18 C 0.91496(19) 0.750000 0.19621(12) 0.0141(5) Uani 1 2 d S T P . .
H18A H 0.919769 0.796207 0.167032 0.017 Uiso 0.5 1 calc R U P . .
H18B H 0.919769 0.703793 0.167032 0.017 Uiso 0.5 1 calc R U P . .
C19 C 1.00838(18) 0.750000 0.24774(12) 0.0138(5) Uani 1 2 d S T P . .
H19 H 1.079034 0.750000 0.223074 0.017 Uiso 1 2 calc R U P . .
C13 C 0.88488(13) 0.60454(10) 0.37510(9) 0.0142(3) Uani 1 1 d . . . . .
H13A H 0.956151 0.593471 0.395810 0.017 Uiso 1 1 calc R U . . .
H13B H 0.864210 0.560019 0.346616 0.017 Uiso 1 1 calc R U . . .
C8 C 0.69691(14) 0.46919(10) 0.41813(10) 0.0172(4) Uani 1 1 d . . . . .
H8A H 0.744396 0.452097 0.455572 0.021 Uiso 1 1 calc R U . . .
H8B H 0.737352 0.463270 0.375205 0.021 Uiso 1 1 calc R U . . .
C20 C 1.00091(13) 0.82208(10) 0.29225(9) 0.0133(3) Uani 1 1 d . . . . .
H20A H 1.006147 0.868679 0.263581 0.016 Uiso 1 1 calc R U . . .
H20B H 1.061958 0.822750 0.324680 0.016 Uiso 1 1 calc R U . . .
C1 C 0.85103(13) 0.57864(10) 0.51757(8) 0.0132(3) Uani 1 1 d . . . . .
H1 H 0.886092 0.529204 0.503697 0.016 Uiso 1 1 calc R U . . .
C7 C 0.66697(13) 0.55421(10) 0.42828(9) 0.0139(3) Uani 1 1 d . . . . .
H7 H 0.623506 0.556199 0.470928 0.017 Uiso 1 1 calc R U . . .
C2 C 0.77418(14) 0.56065(11) 0.57640(9) 0.0174(4) Uani 1 1 d . . . . .
H2A H 0.738454 0.608685 0.591512 0.021 Uiso 1 1 calc R U . . .
H2B H 0.717313 0.524601 0.560863 0.021 Uiso 1 1 calc R U . . .
C9 C 0.59496(15) 0.41870(11) 0.41620(10) 0.0205(4) Uani 1 1 d . . . . .
H9A H 0.615803 0.364746 0.406619 0.025 Uiso 1 1 calc R U . . .
H9B H 0.559112 0.420000 0.460985 0.025 Uiso 1 1 calc R U . . .
C14 C 0.89249(13) 0.67707(10) 0.33146(9) 0.0117(3) Uani 1 1 d . . . . .
C12 C 0.59086(14) 0.58120(11) 0.37189(10) 0.0188(4) Uani 1 1 d . . . . .
H12A H 0.628157 0.577459 0.327675 0.023 Uiso 1 1 calc R U . . .
H12B H 0.570889 0.635730 0.379426 0.023 Uiso 1 1 calc R U . . .
C11 C 0.48849(14) 0.53138(11) 0.37091(10) 0.0211(4) Uani 1 1 d . . . . .
H11A H 0.448269 0.538654 0.413761 0.025 Uiso 1 1 calc R U . . .
H11B H 0.441152 0.548094 0.333262 0.025 Uiso 1 1 calc R U . . .
C6 C 0.94086(14) 0.63311(10) 0.54183(9) 0.0169(4) Uani 1 1 d . . . . .
H6A H 0.991403 0.643550 0.504056 0.020 Uiso 1 1 calc R U . . .
H6B H 0.908576 0.682687 0.556109 0.020 Uiso 1 1 calc R U . . .
C10 C 0.51603(15) 0.44642(11) 0.36227(10) 0.0202(4) Uani 1 1 d . . . . .
H10A H 0.448758 0.415603 0.364910 0.024 Uiso 1 1 calc R U . . .
H10B H 0.548250 0.438248 0.316970 0.024 Uiso 1 1 calc R U . . .
C5 C 1.00319(14) 0.59771(11) 0.60116(9) 0.0188(4) Uani 1 1 d . . . . .
H5A H 1.041728 0.551060 0.585397 0.023 Uiso 1 1 calc R U . . .
H5B H 1.057989 0.634963 0.617385 0.023 Uiso 1 1 calc R U . . .
C4 C 0.92845(15) 0.57624(12) 0.65949(9) 0.0218(4) Uani 1 1 d . . . . .
H4A H 0.898400 0.623733 0.679851 0.026 Uiso 1 1 calc R U . . .
H4B H 0.970537 0.549017 0.694760 0.026 Uiso 1 1 calc R U . . .
C3 C 0.83576(15) 0.52480(12) 0.63574(10) 0.0208(4) Uani 1 1 d . . . . .
H3A H 0.785119 0.516104 0.673797 0.025 Uiso 1 1 calc R U . . .
H3B H 0.865136 0.474200 0.621787 0.025 Uiso 1 1 calc R U . . .
C22 C 0.7821(2) 0.750000 0.01599(14) 0.0202(5) Uani 1 2 d S T P . .
H22 H 0.862061 0.750001 0.008394 0.024 Uiso 1 2 calc R U P . .
C21 C 0.6267(2) 0.750000 0.71280(15) 0.0279(6) Uani 1 2 d S T P . .
H21 H 0.641914 0.749999 0.663107 0.033 Uiso 1 2 calc R U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Pd1 C15 2.093(2) . ?
Pd1 P1 2.2953(4) . ?
Pd1 P1 2.2954(4) 7_575 ?
Pd1 Br1 2.5571(3) . ?
P1 C7 1.8430(17) . ?
P1 C13 1.8432(17) . ?
P1 C1 1.8536(17) . ?
Cl2 C22 1.760(3) . ?
Cl3 C22 1.7684(16) . ?
Cl1 C21 1.757(3) . ?
Cl C21 1.7676(19) . ?
C16 C17 1.530(2) . ?
C16 C14 1.538(2) . ?
C15 C14 1.547(2) 7_575 ?
C15 C14 1.547(2) . ?
C17 C18 1.535(3) . ?
C18 C19 1.539(3) . ?
C19 C20 1.533(2) . ?
C19 C20 1.533(2) 7_575 ?
C13 C14 1.530(2) . ?
C8 C7 1.535(2) . ?
C8 C9 1.535(2) . ?
C20 C14 1.548(2) 7_575 ?
C1 C2 1.533(2) . ?
C1 C6 1.535(2) . ?
C7 C12 1.532(2) . ?
C2 C3 1.530(3) . ?
C9 C10 1.523(3) . ?
C12 C11 1.533(2) . ?
C11 C10 1.524(3) . ?
C6 C5 1.532(2) . ?
C5 C4 1.523(3) . ?
C4 C3 1.527(3) . ?
 
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
C15 Pd1 P1 83.174(12) . . ?
C15 Pd1 P1 83.175(12) . 7_575 ?
P1 Pd1 P1 164.05(2) . 7_575 ?
C15 Pd1 Br1 178.76(6) . . ?
P1 Pd1 Br1 96.914(11) . . ?
P1 Pd1 Br1 96.913(11) 7_575 . ?
C7 P1 C13 110.03(8) . . ?
C7 P1 C1 103.84(8) . . ?
C13 P1 C1 102.44(8) . . ?
C7 P1 Pd1 120.16(6) . . ?
C13 P1 Pd1 104.20(6) . . ?
C1 P1 Pd1 114.84(6) . . ?
C17 C16 C14 110.86(15) . . ?
C14 C15 C14 109.90(19) 7_575 . ?
C14 C15 Pd1 113.74(10) 7_575 . ?
C14 C15 Pd1 113.74(10) . . ?
C16 C17 C16 108.9(2) . 7_575 ?
C16 C17 C18 109.64(13) . . ?
C16 C17 C18 109.64(13) 7_575 . ?
C17 C18 C19 108.93(19) . . ?
C20 C19 C20 109.5(2) . 7_575 ?
C20 C19 C18 109.54(12) . . ?
C20 C19 C18 109.54(13) 7_575 . ?
C14 C13 P1 109.46(11) . . ?
C7 C8 C9 110.78(14) . . ?
C19 C20 C14 110.32(14) . 7_575 ?
C2 C1 C6 109.67(14) . . ?
C2 C1 P1 114.04(12) . . ?
C6 C1 P1 110.27(12) . . ?
C12 C7 C8 110.31(15) . . ?
C12 C7 P1 113.38(12) . . ?
C8 C7 P1 114.84(12) . . ?
C3 C2 C1 110.86(14) . . ?
C10 C9 C8 111.24(15) . . ?
C13 C14 C16 110.06(14) . . ?
C13 C14 C15 110.40(14) . . ?
C16 C14 C15 109.77(14) . . ?
C13 C14 C20 110.08(13) . 7_575 ?
C16 C14 C20 108.00(13) . 7_575 ?
C15 C14 C20 108.48(14) . 7_575 ?
C7 C12 C11 110.07(15) . . ?
C10 C11 C12 111.33(15) . . ?
C5 C6 C1 110.81(15) . . ?
C9 C10 C11 111.75(15) . . ?
C4 C5 C6 111.88(15) . . ?
C5 C4 C3 111.44(15) . . ?
C4 C3 C2 111.75(16) . . ?
Cl2 C22 Cl3 110.18(10) . 7_575 ?
Cl2 C22 Cl3 110.18(10) . . ?
Cl3 C22 Cl3 110.07(15) 7_575 . ?
Cl1 C21 Cl 110.63(11) . . ?
Cl1 C21 Cl 110.63(11) . 7_575 ?
Cl C21 Cl 109.83(17) . 7_575 ?
 
_refine_diff_density_max    0.452
_refine_diff_density_min   -0.815
_refine_diff_density_rms    0.069




