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_4345243
_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         'C60 H72 Br3 N6 P3 Pt3, 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H76 Br3 Cl4 N6 P3 Pt3'
_chemical_formula_weight         1964.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.713(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2931(10)
_cell_length_b                   12.9574(11)
_cell_length_c                   23.1231(14)
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      1.572
_cell_volume                     3335.1(5)
_computing_cell_refinement       'Bruker ApexII Software Suite, 2008'
_computing_data_collection       'Bruker ApexII Software Suite, 2008'
_computing_data_reduction        'Bruker ApexII Software Suite, 2008'
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_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0803
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_max       28
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.444
_diffrn_reflns_theta_min         1.572
_exptl_absorpt_coefficient_mu    8.349
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BLESSING 1995'
_exptl_crystal_colour            red
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_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_restrained_S_all      0.996
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_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^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                4781
_reflns_number_total             6843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00022_si_004.cif
_cod_data_source_block           mn_g346
_cod_depositor_comments
'Adding full bibliography for 4345242--4345243.cif.'
_cod_database_code               4345243
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.483
_shelx_estimated_absorpt_t_max   0.626
_shelx_res_checksum              94593
_shelx_hkl_checksum              48070