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_4324953
_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         'C18 H36 K N2 O6, 0.5(Ag2 H2 P14)'
_chemical_formula_sum            'C18 H37 Ag K N2 O6 P7'
_chemical_formula_weight         741.28
_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             10-06-03
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 103.2695(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4314(6)
_cell_length_b                   10.7798(3)
_cell_length_c                   19.9491(9)
_cell_measurement_reflns_used    7445
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.7
_cell_measurement_theta_min      1.8
_cell_volume                     3020.6(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_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    'isomorphous replacement'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
scan:
    Number of images: 175
               Slice: -60.0000 - 115.0000
         Image width: 1.0000
            Exp time: 1.5000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 59.6267
              2theta: 30.0740
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.5000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 0.0000
                 XTD: 59.6267
              2theta: 30.0740
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.5000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 120.0000
                 XTD: 59.6267
              2theta: 30.0740
scan:
    Number of images: 120
               Slice: -60.0000 - 60.0000
         Image width: 1.0000
            Exp time: 1.5000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -50.0000
                 Phi: 240.0000
                 XTD: 59.6267
              2theta: 30.0740

;
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.023264
_diffrn_orient_matrix_UB_12      -0.033652
_diffrn_orient_matrix_UB_13      -0.058266
_diffrn_orient_matrix_UB_21      0.004359
_diffrn_orient_matrix_UB_22      -0.079478
_diffrn_orient_matrix_UB_23      0.047643
_diffrn_orient_matrix_UB_31      -0.043454
_diffrn_orient_matrix_UB_32      -0.015928
_diffrn_orient_matrix_UB_33      -0.022595
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.208
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37238
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         31.729
_diffrn_reflns_theta_min         1.534
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512.000
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.57
_refine_diff_density_min         -1.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0003
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4667
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1003
_refine_ls_shift/su_max          0.0003574
_refine_ls_shift/su_mean         0.0000147
_refine_ls_structure_factor_coef F
_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: 
 8.04 5.27 5.92 1.62 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1451
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1124
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4667
_reflns_number_total             9950
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      1.76
_oxford_refine_ls_r_factor_ref   0.1003
_oxford_refine_ls_scale          0.840(3)
_oxford_reflns_number_all        6175
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title DIA0086
_cod_data_source_file            ic102516g_si_002_1.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 1 2/n 1 '
_cod_database_code               4324953