Crystal engineering with 1,3,5-triaza-7-phosphaadamantane (PTA): first PTA-driven 3D metal‒organic frameworks
Kirillov, Alexander M.; Wieczorek, Sabina W.; Guedes da Silva, M. Fátima C.; Sokolnicki, Jerzy; Smoleński, Piotr; Pombeiro, Armando J. L.; CrystEngComm 13 (2011) 6329–; doi:10.1039/c1ce05612c

data_7206673
_publ_section_title
;
 Crystal engineering with 1,3,5-triaza-7-phosphaadamantane (PTA): first
 PTA-driven 3D metal--organic frameworks
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              6329
_journal_paper_doi               10.1039/c1ce05612c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C34 H50 Ag4 N12 O8 P4'
_chemical_formula_sum            'C34 H50 Ag4 N12 O8 P4'
_chemical_formula_weight         1310.22
_chemical_name_common
;
catena-((mu4-phenyl-1,2,4,5-tetracarboxylate) -bis(mu2-1,3,5-
triaza-7-phosphaadamantane) -bis(mu3-1,3,5-triaza-7-phosphaadamantane) -
tetrasilver(i)-octahydrate)
;
_chemical_name_systematic
;
catena-((\m4-phenyl-1,2,4,5-tetracarboxylate)
-bis(\m2-1,3,5-triaza-7-phosphaadamantane)
-bis(\m3-1,3,5-triaza-7-phosphaadamantane)
-tetrasilver(I)-octahydrate)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.7040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7271(2)
_cell_length_b                   11.7707(2)
_cell_length_c                   18.2633(4)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.60
_cell_volume                     2491.96(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19953
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.7341
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
;
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.74(3)
_refine_ls_extinction_coef       0.00066(16)
_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   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8918
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                7625
_reflns_number_total             8918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05612c.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7206673