A triangular triplatinum(0) complex with bridging germylene ligands: insertion of alkynes into the Pt‒Ge bond rather than the Pt‒Pt bond
Tanabe, Makoto; Tanaka, Kimiya; Omine, Shumpei; Osakada, Kohtaro; Chemical Communications (Cambridge, United Kingdom) 50 (2014) 6839–6842; doi:10.1039/c4cc00727a

data_7114567
_publ_section_title
;
 A triangular triplatinum(0) complex with bridging germylene ligands:
 insertion of alkynes into the Pt--Ge bond rather than the Pt--Pt bond
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   52
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              6839
_journal_page_last               6842
_journal_paper_doi               10.1039/c4cc00727a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C54 H70 Ge3 O4 P3 Pt3'
_chemical_formula_weight         1679.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.905(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.053(3)
_cell_length_b                   23.593(6)
_cell_length_c                   20.308(5)
_cell_measurement_temperature    90(2)
_cell_volume                     5772(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.1365
_diffrn_reflns_Laue_measured_fraction_full 0.783
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23758
_diffrn_reflns_point_group_measured_fraction_full 0.746
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.177
_diffrn_reflns_theta_min         1.323
_exptl_absorpt_coefficient_mu    8.910
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         9.119
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details
;
 Flack x determined using 3721 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.573(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1231
_refine_ls_number_reflns         15612
_refine_ls_number_restraints     1561
_refine_ls_restrained_S_all      1.281
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.902
_reflns_number_gt                11806
_reflns_number_total             15612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00727a2.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;

2017-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        5772(3)
_cod_original_formula_sum        'C108 H140 Ge6 O8 P6 Pt6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     3358.09
_cod_database_code               7114567
_shelx_estimated_absorpt_t_min   0.269
_shelx_estimated_absorpt_t_max   0.469
_shelxl_version_number           2013-2