Phosphenium Hydride Reduction of [(cod)MX2] (M = Pd, Pt; X = Cl, Br): Snapshots on the Way to Phosphenium Metal(0) Halides and Synthesis of Metal Nanoparticles.
Nickolaus, Jan; Imbrich, Dominik A.; Schlindwein, Simon H.; Geyer, Adrian H.; Nieger, Martin; Gudat, Dietrich; Inorganic chemistry 56 (2017) 3071–3080; doi:10.1021/acs.inorgchem.7b00022

data_4345242
_publ_section_title
;
 Phosphenium Hydride Reduction of [(cod)MX2] (M = Pd, Pt; X = Cl, Br):
 Snapshots on the Way to Phosphenium Metal(0) Halides and Synthesis of
 Metal Nanoparticles.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3071
_journal_page_last               3080
_journal_paper_doi               10.1021/acs.inorgchem.7b00022
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C30 H60 Cl3 N6 P3 Pt3, 2(C4 H8 O)'
_chemical_formula_sum            'C58 H87 Cl N4 P2 Pt'
_chemical_formula_weight         1132.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1399(15)
_cell_length_b                   16.345(2)
_cell_length_c                   23.168(3)
_cell_measurement_reflns_used    8156
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.413
_cell_measurement_theta_min      1.525
_cell_volume                     5733.2(12)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
_computing_molecular_graphics    'SHELXS plus XP (Sheldrick, 1991)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa ApexII Duo'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41272
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         1.525
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '*BLESSING 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.065
_refine_diff_density_max         2.601
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
 Flack x determined using 2785 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11704
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0528
_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/[\s^2^(Fo^2^)+(0.0245P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                8156
_reflns_number_total             11704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00022_si_003.cif
_cod_data_source_block           mn_g316
_cod_depositor_comments
'Adding full bibliography for 4345242--4345243.cif.'
_cod_database_code               4345242
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              98820
_shelx_hkl_checksum              77733