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_4345571
_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            'C38 H76 Cl3 N6 O2 P3 Pt3'
_chemical_formula_weight         1433.57
_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   geom
_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                   14.1385(7)
_cell_length_b                   16.4928(8)
_cell_length_c                   21.4412(10)
_cell_measurement_reflns_used    10756
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.332
_cell_measurement_theta_min      1.725
_cell_volume                     4999.7(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43924
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         1.725
_exptl_absorpt_coefficient_mu    8.667
_exptl_absorpt_correction_T_max  0.5683
_exptl_absorpt_correction_T_min  0.1755
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details
;
 Flack x determined using 4399 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         12241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                10756
_reflns_number_total             12241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00022_si_002.cif
_cod_data_source_block           mn_g242
_cod_database_code               4345571
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.266
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              5124
_shelx_hkl_checksum              '13940 '