Coordination of Tri-Substituted Nona-Germanium Clusters to Cu(I) and Pd(0).
Li, Feng; Sevov, Slavi C.; Inorganic chemistry 54 (2015) 8121–8125; doi:10.1021/acs.inorgchem.5b01371

data_4344046
_publ_section_title
;
 Coordination of Tri-Substituted Nona-Germanium Clusters to Cu(I) and
 Pd(0).
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8121
_journal_page_last               8125
_journal_paper_doi               10.1021/acs.inorgchem.5b01371
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'2(K C18 N2 O6 H36), (Ge18 Si24 C54 H162 Pd), 2(C2 N H3)'
_chemical_formula_sum            'C47 H120 Ge9 K N3 O6 Pd0.5 Si12'
_chemical_formula_weight         1906.14
_chemical_name_common            (Kcrypt)2{(Ge9R3)PdGe9R3)}.2MeCN
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                64.778(2)
_cell_angle_beta                 79.495(3)
_cell_angle_gamma                89.554(3)
_cell_formula_units_Z            2
_cell_length_a                   15.5519(12)
_cell_length_b                   16.8841(14)
_cell_length_c                   18.1601(15)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.30
_cell_volume                     4228.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19277
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_min         1.264
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            black-brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1938
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.702
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         19277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0336P)^2^+5.9265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15529
_reflns_number_total             19277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01371_si_002.cif
_cod_data_source_block           LF091_0m
_cod_depositor_comments
'Adding full bibliography for 4344046--4344047.cif.'
_cod_original_formula_sum        'C47 H120 Ge9 K N3 O6 Pd0.50 Si12'
_cod_database_code               4344046
_shelx_estimated_absorpt_t_min   0.373
_shelx_estimated_absorpt_t_max   0.621
_shelxl_version_number           2013-4
_shelx_res_checksum              85255
_shelx_hkl_checksum              84017