Robust 2D Coordination Networks from a Two-Step Assembly Process with Predesigned Silver Cyclic Dimers and Hexamethylenetetramine
Durá, Gema; Carrión, M. Carmen; Jalón, Félix A.; Manzano, Blanca R.; Rodríguez, Ana M.; Mereiter, Kurt; Crystal Growth & Design 15 (2015) 3321–; doi:10.1021/acs.cgd.5b00428

data_4513275
_publ_section_title
;
 Robust 2D Coordination Networks from a Two-Step Assembly Process with
 Predesigned Silver Cyclic Dimers and Hexamethylenetetramine
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3321
_journal_paper_doi               10.1021/acs.cgd.5b00428
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C42 H45 Ag3 N19, 3(Cl O4) '
_chemical_formula_sum            'C42 H45 Ag3 Cl3 N19 O12'
_chemical_formula_weight         1437.93
_chemical_name_common            '1666 bm AgClO4-eggcrate squeezed'
_chemical_name_systematic
; 
Silver perchlorate / 4-[di(pyrazol-1-yl)methyl]pyridine / hexamethylene-
teramine 3:3:1 coordination polymer, 2-dimensional, with unknown solvent 
squeezed and not contained in chemical formula and quantities 
derived thereof.
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.5686(5)
_cell_length_b                   22.5686(5)
_cell_length_c                   22.2724(5)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.28
_cell_volume                     9824.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41827
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    1.074
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS, V. 2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4308
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
Compound is a 2-dimensional coordination polymer with 
layers of egg-crate like structure parallel to 
(001) of the trigonal unit cell (R-lattice). The compound
contains large cavities occupied by disordered solvent 
that was squeezed with program PLATON.
Total Potential Solvent Accessible Void Volume is 2291 Ang^3 
or 23.3% of the unit cell volume.
Electron Count / Cell is 544 and is not included in D(calc), 
F000 & Mol.Wght.
;
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1221P)^2^+13.8562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2277
_reflns_number_gt                2300
_reflns_number_total             3307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00428_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'trigonal ' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513274--4513276.cif.
;
_cod_original_sg_symbol_Hall     '-R 3 2" '
_cod_original_sg_symbol_H-M      'R -3 m '
_cod_database_code               4513275