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_7008794
_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         'C12 H17 N7 O3'
_chemical_formula_sum            'C12 H18 N8 O6'
_chemical_formula_weight         370.34
_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             2005-07-20T19:37:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.169(14)
_cell_angle_beta                 90.492(11)
_cell_angle_gamma                108.333(14)
_cell_formula_units_Z            1
_cell_length_a                   4.8927(7)
_cell_length_b                   7.4395(14)
_cell_length_c                   12.6052(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      10.05
_cell_measurement_wavelength     0.71073
_cell_volume                     413.51(12)
_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 1
_diffrn_measured_fraction_theta_max 1
_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      -0.081081
_diffrn_orient_matrix_UB_12      -0.143434
_diffrn_orient_matrix_UB_13      -0.046494
_diffrn_orient_matrix_UB_21      0.059445
_diffrn_orient_matrix_UB_22      0.037457
_diffrn_orient_matrix_UB_23      -0.068367
_diffrn_orient_matrix_UB_31      0.191937
_diffrn_orient_matrix_UB_32      -0.016319
_diffrn_orient_matrix_UB_33      0.012083
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0091
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2503
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.7
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             194
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.1306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                1872
_reflns_number_total             2404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508260a.txt
_cod_data_source_block           pm80
_cod_original_cell_volume        413.51(11)
_cod_database_code               7008794
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1