#============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Simona Galli' _publ_contact_author_address ; Dipartimento di Scienza e Alta Tecnologia, Universita' dell'Insubria, Via Valleggio 9, 22100 Como, Italy ; _publ_contact_author_email 'simona.galli@uninsubria.it' _publ_contact_author_fax ? _publ_contact_author_phone '+39-031_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 ; Novel Coordination Polymers with (Pyrazolato)-based Tectons: Catalytic Activity in the Peroxidative Oxidation of Alcohols and Cyclohexane ; # 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 'Timokin, Ivan' ; School of Farmacy, Chemistry Section University of Camerino Via S. Agostino 1, 62032 Camerino, Italy ; 'Pettinari, Claudio' ; School of Farmacy, Chemistry Section University of Camerino Via S. Agostino 1, 62032 Camerino, Italy ; 'Marchetti, Fabio' ; School of Science and Technology, Chemistry Section University of Camerino Via S. Agostino 1, 62032 Camerino, Italy ; 'Pettinari, Riccardo' ; School of Farmacy, Chemistry Section University of Camerino Via S. Agostino 1, 62032 Camerino, Italy ; 'Condello, Francesca' ; School of Farmacy, Chemistry Section University of Camerino Via S. Agostino 1, 62032 Camerino, Italy ; 'Galli, Simona' ; Dipartimento di Scienza e Alta Tecnologia, Università degli Studi dell'Insubria, Via Valleggio 11, 22100 Como, Italy ; 'Alegria, Elisabete C.B.A.' ; Centro de Química Estrutural, Instituto Superior Técnico Universidade de Lisboa Av. Rovisco Pais, 1049-001 Lisboa, Portugal ; 'Martins, Luísa M.D.R.S.' ; Centro de Química Estrutural, Instituto Superior Técnico Universidade de Lisboa Av. Rovisco Pais, 1049-001 Lisboa, Portugal ; 'Pombeiro, Armando J.L.' ; Centro de Química Estrutural, Instituto Superior Técnico Universidade de Lisboa Av. Rovisco Pais, 1049-001 Lisboa, Portugal ; #============================================================================== #data_Compound_3Cd _chemical_name_systematic ; catena-(bis(4-pyrazolato)methane)-cd(ii) ; _chemical_name_common ? _chemical_formula_moiety 'C14 H12 Cd2 N8' _chemical_formula_structural 'Cd2 (C14 H12 N8)' _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C14 H12 Cd2 N8' _chemical_formula_weight 517.13 _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)' #============================================================================== # 1.5. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system 'monoclinic' _space_group_name_H-M_alt 'P2(1)/a' _space_group_name_Hall '?' loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x+1/2, y+1/2, -z' 'x, y, z' 'x+1/2, -y+1/2, z' _cell_length_a 14.77452(98) _cell_length_b 15.2460(11) _cell_length_c 9.30985(69) _cell_angle_alpha 90 _cell_angle_beta 79.5039(58) _cell_angle_gamma 90 _cell_volume 2061.97(26) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.67 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 10 # perpendicular to # equatorial plane _pd_spec_size_equat 10 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.05 # 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 ? _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 'Nickel 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 D8 Commander' _computing_cell_refinement 'TOPAS-R' _computing_data_reduction ? _computing_structure_solution 'TOPAS-R' _computing_structure_refinement 'TOPAS-R' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 1.7. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The use of a rigid body description for the two, crystallographically independent bis(4-pyrazolato)methane ligands does not allow the derivation of statistically meaningful s.u.'s for their atoms. S.u.'s are available only for the position of their center of mass (X, Y, Z), their rotation angles (RX, RY, RZ) and the torsion angles (T1, T2) around the C-C exocyclic bonds: Ligand I: (X, Y, Z) = (-0.0256(6), 0.4133(6), 0.7211(9)) (RX, RY, RZ) = (-104.7(2), -97.215(3), -130.9(2)) (T1, C1-C2) = 168(1) (T2, C1-C5) = 205(1) Ligand II: (X, Y, Z) = (0.8033(6), 0.9214(6), 0.2803(9)) (RX, RY, RZ) = (273.6(3), -182.8(2), -313.2(3)) (T1, C1-C2) = 227(2) (T2, C1-C5) = -219(1) for the rigid body described as: z_matrix C1 z_matrix C2 C1 =r1 z_matrix C3 C2 =r2 C1 126 z_matrix H3 C3 =r3 C2 126 C1 0 z_matrix N1 C3 =r2 C2 108 C1 180 z_matrix N2 N1 =r2 C3 108 C2 0 z_matrix C4 N2 =r2 N1 108 C3 0 z_matrix H4 C4 =r3 N2 126 N1 180 z_matrix H11 C1 =r4 C2 109.5 C3 180 z_matrix H12 C1 =r4 C2 109.5 H11 128 z_matrix C5 C1 =r1 C2 =a1 H11 240 z_matrix C6 C5 =r1 C1 126 C2 180 z_matrix H6 C6 =r3 C5 126 C1 0 z_matrix N3 C6 =r2 C5 108 C1 180 z_matrix N4 N3 =r2 C6 108 C5 0 z_matrix C7 N4 =r2 N3 108 C6 0 z_matrix H7 C7 =r3 N4 126 N3 180 r1 1.50 refined r2 1.36 fixed r3 0.95 fixed r4 1.10 fixed a1 113.0 refined ; # 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 0.051 _pd_proc_ls_prof_wR_factor 0.067 _pd_proc_ls_prof_wR_expected 0.033 _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 58 _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 8 _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 ? #============================================================================== # 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cd1 Cd 4 -0.26050(41) 0.29652(26) 0.29949(59) 1 5.00(11) Cd2 Cd 4 -0.50259(39) 0.73862(34) 0.77572(57) 1 5.00(11) C1 C 4 -0.02555 0.41327 0.72114 1 7.00(11) C2 C 4 0.02550288 0.3511399 0.6101463 1 7.00(11) C3 C 4 -0.009903933 0.3086872 0.5043902 1 7.00(11) H3 H 4 -0.07131245 0.3131753 0.4878424 1 7.00(11) N1 N 4 0.058035 0.2586812 0.4264828 1 7.00(11) N2 N 4 0.1354304 0.2702286 0.4840895 1 7.00(11) C4 C 4 0.1153244 0.3273712 0.5975998 1 7.00(11) H4 H 4 0.1567497 0.3472022 0.657593 1 7.00(11) H11 H 4 -0.09162744 0.4309407 0.6903263 1 7.00(11) H12 H 4 -0.02970698 0.3854526 0.8311683 1 7.00(11) C5 C 4 0.02620981 0.4966704 0.7341525 1 7.00(11) C6 C 4 0.1277826 0.5100297 0.6858204 1 7.00(11) H6 H 4 0.1706252 0.4671557 0.6415946 1 7.00(11) N3 N 4 0.1477746 0.5942956 0.7164279 1 7.00(11) N4 N 4 0.0680376 0.6342624 0.7791655 1 7.00(11) C7 C 4 -0.001234515 0.5746973 0.7873319 1 7.00(11) H7 H 4 -0.064337 0.5849266 0.8264644 1 7.00(11) C1a C 4 0.80335 0.92138 0.28032 1 7.00(11) C2a C 4 0.8195358 0.018023 0.2590929 1 7.00(11) C3a C 4 0.9026551 0.057642 0.2175109 1 7.00(11) H3a H 4 0.9606592 0.028968 0.1968088 1 7.00(11) N1a N 4 0.888158 0.145517 0.2107689 1 7.00(11) N2a N 4 0.7960791 0.160208 0.2481842 1 7.00(11) C4a C 4 0.7536682 0.081413 0.27805 1 7.00(11) H4a H 4 0.6893286 0.072258 0.3070609 1 7.00(11) H11a H 4 0.8517527 0.8945808 0.3458873 1 7.00(11) H12a H 4 0.7299591 0.9093907 0.3229835 1 7.00(11) C5a C 4 0.8165753 0.8714264 0.1392318 1 7.00(11) C6a C 4 0.7416699 0.8411945 0.06165681 1 7.00(11) H6a H 4 0.6775247 0.8503232 0.09325591 1 7.00(11) N3a N 4 0.7817071 0.7984212 -0.06185666 1 7.00(11) N4a N 4 0.8743657 0.7993962 -0.06785753 1 7.00(11) C7a C 4 0.8915946 0.842772 0.05194721 1 7.00(11) H7a H 4 0.9505632 0.8531961 0.07557307 1 7.00(11)