#============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. Simona Galli' _publ_contact_author_address ; Dipartimento di Scienza e Alta Tecnologia, Università dell'Insubria, Via Valleggio, 11 - 22100 Como - Italy ; _publ_contact_author_email 'simona.galli@uninsubria.it' _publ_contact_author_fax '+39-031-2386630' _publ_contact_author_phone '+39-958-2386627' _publ_requested_journal 'Crystal Growth and Design' _publ_requested_category 'FA' _publ_contact_letter ; ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Enlarging an isoreticular family: 3,3',5,5'-tetramethyl-4,4'-bipyrazolato-based porous coordination polymers ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Tabacaru, Aurel' ; Scuola di Scienze del Farmaco e dei Prodotti della Salute, Università di Camerino, Via S. Agostino 1 - 62032 Camerino - Italy. ; 'Pettinari, Claudio' ; Scuola di Scienze del Farmaco e dei Prodotti della Salute, Università di Camerino, Via S. Agostino 1 - 62032 Camerino - Italy. ; 'Timokin, Ivan' ; Scuola di Scienze e Tecnologie, Università di Camerino, Via S. Agostino 1 - 62032 Camerino - Italy. ; 'Marchetti, Fabio' ; Scuola di Scienze e Tecnologie, Università di Camerino, Via S. Agostino 1 - 62032 Camerino - Italy. ; 'Carrasco-Marín, Francisco' ; Departamento de Química Inorgánica, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada - Spain. ; 'Maldonado-Hódar, Francisco José' ; Departamento de Química Inorgánica, Universidad de Granada, Av. Fuentenueva s/n, 18071 Granada - Spain. ; 'Masciocchi, Norberto' ; Dipartimento di Scienze Chimiche e Ambientali, Università degli Studi dell'Insubria, Via Valleggio 11, 22100 Como - Italy. ; 'Galli, Simona' ; Dipartimento di Scienze Chimiche e Ambientali, Università degli Studi dell'Insubria, Via Valleggio 11, 22100 Como - Italy. ; #============================================================================== data_Compound3 _chemical_name_systematic ; catena-3,3',5,5'-tetramethyl-4,4'-bipyrazolato-cd(ii) ; _chemical_name_common ? _chemical_formula_moiety 'C10 H12 Cd1 N4' _chemical_formula_structural 'Cd1 (C10 H12 N4)' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C10 H12 Cd1 N4' _chemical_formula_weight 300.63 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description # _atom_type_scat_dispersion_real # _atom_type_scat_dispersion_imag _atom_type_scat_source C C 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' Cd Cd 'International Tables for Crystallography (Vol. IV)' N N 'International Tables for Crystallography (Vol. IV)' #============================================================================== _space_group_crystal_system 'hexagonal' _space_group_name_H-M_alt 'P6122' _space_group_name_Hall '?' loop_ _symmetry_equiv_pos_as_xyz '-x, -x+y, -z-1/3' '-x, -y, z+1/2' '-x+y, -x, z-1/3' '-x+y, y, -z+1/2' '-y, -x, -z-1/6' '-y, x-y, z+1/3' 'y, -x+y, z-1/6' 'y, x, -z+1/3' 'x-y, -y, -z' 'x-y, x, z+1/6' 'x, y, z' 'x, x-y, -z+1/6' _cell_length_a 9.132637(70) _cell_length_b 9.132637(70) _cell_length_c 23.09972(24) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1668.514(31) _cell_formula_units_Z 6 _cell_measurement_temperature 298 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.79 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 15 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.2 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour white # use ICDD colour descriptions # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # 1.6. EXPERIMENTAL DATA _exptl_special_details ; ? ; # This following item is used to identify the equipment used to record the # powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _diffrn_ambient_temperature 298 _diffrn_source_target Cu _diffrn_source_type 'sealed X-ray tube' _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_detector_type 'Bruker Lynxeye linear PSD' _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength CuK\a~1~ 1.54056 CuK\a~2~ 1.54439 _diffrn_radiation_monochromator 'Ni filter' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5001 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 105 _pd_meas_2theta_range_inc 0.02 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'Bruker AXS Commander' _computing_cell_refinement 'TOPAS-R' _computing_data_reduction ? _computing_structure_solution 'TOPAS-R' _computing_structure_refinement 'TOPAS-R' _computing_molecular_graphics 'Schakal99' _computing_publication_material 'TOPAS-R' #============================================================================== # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The crystallographically independent portion of the organic ligand was described, through the z-matrix formalism, by the following rigid body: z_matrix Du z_matrix C1 Du =r1/2; z_matrix C2 C1 =r3; Du 126 z_matrix C3 C2 =r2; C1 126 Du 0 z_matrix H31 C3 =r4; C2 109.5 C1 0 z_matrix H32 C3 =r4; C2 109.5 C1 120 z_matrix H33 C3 =r4; C2 109.5 C1 -120 z_matrix N1 C2 =r3; C1 108 Du 180 z_matrix C6 Du =r1/2; C1 180 C2 0 z_matrix C7 C6 =r3; Du 126 C2 0 z_matrix C8 C7 =r2; C6 126 Du 0 z_matrix H81 C8 =r4; C7 109.5 C6 0 z_matrix H82 C8 =r4; C7 109.5 C6 120 z_matrix H83 C8 =r4; C7 109.5 C6 -120 z_matrix N3 C7 =r3; C6 108 Du 180 r1 = 1.54 r2 = 1.54 r3 = 1.36 r4 = 0.95 Du = centre of mass The centre of mass lies in (0, -0.5953(3), 1/6), and the whole ligand is rotated, with respect to the unit cell axis a, b, and c, of (90, 0, 30) deg, respeciively. The two five-membered rings are rotated, with respect to the C-C exocyclic bond, by -315.7(2) and 82.5(2) deg. ; # The next three items are given as text _pd_proc_ls_profile_function 'fundamental parameters approach' _pd_proc_ls_background_function 'Chebychev polynomial' _pd_proc_ls_pref_orient_corr ? _pd_proc_ls_prof_R_factor 0.059 _pd_proc_ls_prof_wR_factor 0.084 _pd_proc_ls_prof_wR_expected 0.007 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme '1/[Y~i~]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 24 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? # The following item is 'CHI squared' _refine_ls_goodness_of_fit_all ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 10 _pd_proc_2theta_range_max 105 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540562 1.544390 _pd_block_diffractogram_id ? # The id used for the block # containing the powder # pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Cd Cd 6 0.062748(84) 0.12550(17) 0.25 1 0.811(39) C1 C 6 0 -0.6795828 -0.1666667 0.5 2.811(39) C2 C 12 0.09955336 -0.717337 -0.1333972 1 2.811(39) C3 C 12 0.2320749 -0.598968 -0.08911017 1 2.811(39) H31 H 12 0.2557873 -0.4863435 -0.09529508 1 2.811(39) H32 H 12 0.1893776 -0.6335707 -0.05102901 1 2.811(39) H33 H 12 0.3329262 -0.603866 -0.09364769 1 2.811(39) N1 N 12 0.06152736 -0.877978 -0.146105 1 2.811(39) C6 C 6 0 -0.5109568 -0.1666667 0.5 2.811(39) C7 C 12 0.01827063 -0.4142906 -0.2138851 1 2.811(39) C8 C 12 0.04259178 -0.4542383 -0.2767404 1 2.811(39) H81 H 12 0.05732017 -0.5501034 -0.2772564 1 2.811(39) H82 H 12 -0.05418325 -0.4773798 -0.2989624 1 2.811(39) H83 H 12 0.139663 -0.3599098 -0.2928319 1 2.811(39) N3 N 12 0.01129187 -0.276152 -0.1958493 1 2.811(39)