From recovered metal waste to high-performance palladium catalysts
Jantan, Khairil Anuar; Kwok, Chuek Yee; Chan, Kuang Wen; Marchiò, Luciano; White, Andrew J. P.; Deplano, Paola; Serpe, Angela; Wilton-Ely, James; Green Chemistry  (2017) –; doi:10.1039/C7GC02678A

data_7229601
_publ_section_title
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 From recovered metal waste to high-performance palladium catalysts
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/C7GC02678A
_journal_year                    2017
_chemical_formula_moiety         'C90 H78 N2 P4 Pd2 S4, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C94 H88 F12 N2 O P6 Pd2 S4'
_chemical_formula_weight         2016.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-28 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5109(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.0045(5)
_cell_length_b                   10.85381(18)
_cell_length_c                   26.7343(4)
_cell_measurement_reflns_used    7869
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.2840
_cell_measurement_theta_min      4.2650
_cell_volume                     9182.0(3)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14026
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.744
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.606
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       tablets
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.455(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         9980
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0373
_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/[\s^2^(Fo^2^)+(0.0626P)^2^+5.7330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                9490
_reflns_number_total             9980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7gc02678a2.cif
_cod_data_source_block           4
_cod_database_code               7229601
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              83321
_shelx_fab_checksum              34575