Solventless Supramolecular Chemistry via Vapor Diffusion of Volatile Small Molecules upon a New Trinuclear Silver(I)-Nitrated Pyrazolate Macrometallocyclic Solid: An Experimental/Theoretical Investigation of the Dipole/Quadrupole Chemisorption Phenomena
Rossana Galassi; Simone Ricci; Alfredo Burini; Alceo Macchioni; Luca Rocchigiani; Fabio Marmottini; Sammer M. Tekarli; Vladimir N. Nesterov; Mohammad A. Omary; Inorganic Chemistry 52 (2013) 14124–14137; doi:10.1021/ic401948p

data_4336996
_publ_section_title
;
 Solventless Supramolecular Chemistry via Vapor Diffusion of Volatile
 Small Molecules upon a New Trinuclear Silver(I)-Nitrated Pyrazolate
 Macrometallocyclic Solid: An Experimental/Theoretical Investigation of
 the Dipole/Quadrupole Chemisorption Phenomena
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14124
_journal_page_last               14137
_journal_paper_doi               10.1021/ic401948p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C12 H4 Ag3 N16 O16, Ag H6 N2 '
_chemical_formula_sum            'C12 H10 Ag4 N18 O16'
_chemical_formula_weight         1093.86
_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                90.0320(10)
_cell_angle_beta                 91.9370(10)
_cell_angle_gamma                98.991(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5731(3)
_cell_length_b                   12.2440(5)
_cell_length_c                   13.8489(5)
_cell_measurement_reflns_used    9355
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.23
_cell_volume                     1435.00(9)
_computing_cell_refinement       'APEX2 (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2007)'
_computing_data_reduction        'APEX2 (Bruker-AXS, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18037
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  0.8706
_exptl_absorpt_correction_T_min  0.4482
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.532
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00056(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0199
_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 w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                5731
_reflns_number_total             6355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401948p_si_003.cif
_cod_data_source_block           str0290
_cod_database_code               4336996