Heteroatomic Molecular Clusters Derived from Group 15 Zintl Ion Cages: Synthesis and Isolation of [M2(HP7)2]2- (M = Ag, Au), Two Novel Cluster Anions Exhibiting Metallophilic Interactions
Caroline M. Knapp; Charlotte S. Jackson; Joseph S. Large; Amber L. Thompson; Jose M. Goicoechea; Inorganic Chemistry 50 (2011) 4021–4028; doi:10.1021/ic102516g

data_4324955
_publ_contact_author             'Jos\'e M. Goicoechea'
_publ_contact_author_email       jose.goicoechea@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 275961'
_publ_section_title
;
 Heteroatomic Molecular Clusters Derived from Group 15 Zintl Ion Cages:
 Synthesis and Isolation of [M2(HP7)2]2- (M = Ag, Au), Two Novel Cluster
 Anions Exhibiting Metallophilic Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4021
_journal_page_last               4028
_journal_paper_doi               10.1021/ic102516g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '2(C18 H36 K N2 O6), Au2 H2 P14'
_chemical_formula_sum            'C36 H74 Au2 K2 N4 O12 P14'
_chemical_formula_weight         1660.76
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-05-21
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 102.8771(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4130(2)
_cell_length_b                   10.8462(2)
_cell_length_c                   19.9351(4)
_cell_measurement_reflns_used    152841
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3038.00(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.113
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66526
_diffrn_reflns_theta_full        26.924
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         5.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.383
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       lath
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.25
_refine_diff_density_min         -2.09
_refine_ls_extinction_coef       210(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9335
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6904
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.0006491
_refine_ls_shift/su_mean         0.0000158
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1417
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1417
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                5018
_reflns_number_total             6906
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0819
_oxford_refine_ls_scale          0.08361(4)
_oxford_reflns_number_all        6904
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6273
_cod_data_source_file            ic102516g_si_002_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 1 2/n 1 '
_cod_original_formula_sum        'C18 H37 Au1 K1 N2 O6 P7'
_cod_database_code               4324955