A coordination network containing non-coordinating polyoxometalate clusters as counterions
Johnson, Bret J. S.; Geers, Sarah A.; Brennessel, William W.; Young, Jr., Victor G.; Stein, Andreas; Dalton Transactions  (2003) 4678–; doi:10.1039/b309453g

data_7013512
_publ_section_title
;
 A coordination network containing non-coordinating polyoxometalate
 clusters as counterions
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4678
_journal_paper_doi               10.1039/b309453g
_journal_year                    2003
_chemical_formula_moiety         'C68 H101 As4 Co2 Mo12 N9 O60 S7'
_chemical_formula_sum            'C68 H101 As4 Co2 Mo12 N9 O60 S7'
_chemical_formula_weight         3797.82
_chemical_name_common            01141
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.469(1)
_cell_angle_beta                 83.772(1)
_cell_angle_gamma                80.423(1)
_cell_formula_units_Z            2
_cell_length_a                   15.5503(8)
_cell_length_b                   16.3975(9)
_cell_length_c                   25.675(1)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    173(2)
_cell_volume                     6411.1(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41036
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    2.608
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.820829
_exptl_absorpt_correction_type   multiscans
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat block'
_exptl_crystal_F_000             3708
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.168
_refine_diff_density_min         -2.301
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1364
_refine_ls_number_reflns         22584
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0359P)^2^+0.0000sin\q/\l]
where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                11711
_reflns_number_total             22584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309453g.txt
_cod_data_source_block           01141
_cod_original_cell_volume        6411.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013512