Ag(i) complexes with alkylidene-bis(2-aminopyrimidines) as building units for discrete metallomacrocyclic frames. A structural and solution study
García-Raso, Angel; Fiol, Juan J.; Tasada, Andrés; Albertí, Francisca M.; Molins, Elies; Basallote, Manuel G.; Máñez, María A.; Fernández-Trujillo, María J.; Sánchez, David; Dalton Transactions  (2005) 3763–; doi:10.1039/b508260a

data_7008797
_publ_section_title
;
 Ag(i) complexes with alkylidene-bis(2-aminopyrimidines) as building
 units for discrete metallomacrocyclic frames. A structural and
 solution study
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3763
_journal_paper_doi               10.1039/b508260a
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 Ag1 N12'
_chemical_formula_sum            'C24 H34 Ag2 N16 O12'
_chemical_formula_weight         954.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-11-03T18:31:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.53(5)
_cell_angle_beta                 84.45(4)
_cell_angle_gamma                70.23(4)
_cell_formula_units_Z            1
_cell_length_a                   7.878(7)
_cell_length_b                   9.067(5)
_cell_length_c                   13.252(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      14
_cell_measurement_wavelength     0.71073
_cell_volume                     854.2(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.027104
_diffrn_orient_matrix_UB_12      -0.066512
_diffrn_orient_matrix_UB_13      0.074515
_diffrn_orient_matrix_UB_21      -0.053006
_diffrn_orient_matrix_UB_22      0.100709
_diffrn_orient_matrix_UB_23      0.024627
_diffrn_orient_matrix_UB_31      -0.12114
_diffrn_orient_matrix_UB_32      -0.014859
_diffrn_orient_matrix_UB_33      0.005923
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3160
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.6
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.474
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+1.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.097
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                2776
_reflns_number_total             3016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508260a.txt
_cod_data_source_block           pm72
_cod_database_code               7008797
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1