Tri-, hepta- and octa-nuclear Ag(i) complexes derived from 2-pyridyl-functionalized tris(amido)phosphate ligand.
Gupta, Arvind K.; Steiner, Alexander; Boomishankar, Ramamoorthy; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9753–9759; doi:10.1039/c2dt30241a

data_7019713
_publ_section_title
;
 Tri-, hepta- and octa-nuclear Ag(i) complexes derived from
 2-pyridyl-functionalized tris(amido)phosphate ligand.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9753
_journal_page_last               9759
_journal_paper_doi               10.1039/c2dt30241a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'C60 H54 Ag8 N24 O4 P4 4+, (Cl O4 1-)4, (C H4 O)5, (H2 O)3'
_chemical_formula_sum            'C65 H80 Ag8 Cl4 N24 O28 P4'
_chemical_formula_weight         2774.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.737(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.075(3)
_cell_length_b                   13.2864(7)
_cell_length_c                   27.6363(15)
_cell_measurement_reflns_used    147
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.10
_cell_volume                     18018.2(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'Omega and phi 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_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            104100
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
The unit cell contains 4 perchlorate ions, 5 methanol and three water molecules
which have been treated as a diffuse contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         15842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                9115
_reflns_number_total             15842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30241a.txt
_cod_data_source_block           compound3a_new_squeeze
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        18018.2(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7019713