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_4324954
_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), Ag2 H2 P14'
_chemical_formula_sum            'C36 H74 Ag2 K2 N4 O12 P14'
_chemical_formula_weight         1482.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.3363(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7536(1)
_cell_length_b                   27.0054(2)
_cell_length_c                   10.6651(1)
_cell_measurement_reflns_used    58107
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3094.63(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.029
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57032
_diffrn_reflns_theta_full        27.467
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         5.157
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9505
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.0006710
_refine_ls_shift/su_mean         0.0000310
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 7.76 11.2 6.42 2.69 0.570 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0783
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0783
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -34
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                5094
_reflns_number_total             7032
_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   0.0582
_oxford_refine_ls_scale          0.14511(4)
_oxford_reflns_number_all        7032
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6272
_cod_data_source_file            ic102516g_si_002_2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C18 H37 Ag1 K1 N2 O6 P7'
_cod_database_code               4324954