Electronic supplementary material (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.-H.Her P.W.Stephens Q.Zhu K.J.Nelson J.S.Miller _publ_contact_author_name 'Joel S. Miller' _publ_contact_author_email jsmiller@chem.utah.edu data_C4H6BCrF5N2 _database_code_depnum_ccdc_archive 'CCDC 675736' # 5. CHEMICAL DATA _chemical_name_systematic ; Bis(acetonitrile)-mu-fluoro-mu-tetrafluoroboratechromium(II) ; _chemical_name_common Bis(acetonitrile)-mu-fluoro-mu-tetrafluoroboratechromium(ii) _chemical_formula_moiety 'C4 H6 B Cr F5 N2' _chemical_formula_structural 'Cr F (N C (C H3))2 B F4' _chemical_formula_analytical ? _chemical_formula_sum 'C4 H6 B Cr F5 N2' _chemical_formula_weight ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' 1 'x, y, z' 2 '-x, y, -z+1/2' 3 '-x, -y, -z' 4 'x, -y, z+1/2' 5 'x+1/2, y+1/2, z' 6 '-x+1/2, y+1/2, -z+1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.2555(6) _cell_length_b 10.4744(5) _cell_length_c 7.2559(4) _cell_angle_alpha 90 _cell_angle_beta 83.019(5) _cell_angle_gamma 90 _cell_volume 924.5(1) _cell_formula_units_Z 4 _cell_measurement_temperature 300 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu 11.8191 # cm^-1 @ E_ph = 17699 eV _exptl_absorpt_correction_type none # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The 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 ; X16C, National Synchrotron Light Source, Brookhaven National Laboratory ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; NIST standard reference material 1976(sintered plate of Al2O3) Well-isolated 7 reflections were used to calibrate wavelength and detector zero. ; _diffrn_ambient_temperature 300 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type 'Huber diffractometer' _diffrn_detector 'NaI scintillation counter' _diffrn_detector_type ? # make or model of detector _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. _diffrn_radiation_wavelength 0.700486 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 8601 _pd_meas_2theta_range_min 2.000 _pd_meas_2theta_range_max 45.000 _pd_meas_2theta_range_inc .005 # 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 ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Acetonitrile(NCMe) molecule is defined as rigid body in order to ride the three hydrogen atoms of methyl group on the carbon atom using z-matrix function implemented in TOPAS-Academic. The same isotropic displacement parameters are assigned to the atoms that belong to the same molecule (e.g., BF4 and NCMe). Individual e.s.d. of atomic coordinates are not reported if they are treated as rigid body (i.e., the NCMe molecule). The esd's listed for fractional coordinates and isotropic displacement parameters are those reported by the least squares refinement, and are estimates of purely statistical uncertainty. We have increased the quoted uncertainties derived bond lengths/angles by a factor of 5, to obtain numbers which are more appropriate estimates of the confidence limits. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=330 in TOPAS-Academic ; _pd_proc_ls_background_function ; Chebyshev polynomial with 41 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.027 # 2.698(%) _pd_proc_ls_prof_wR_factor 0.034 # 3.441(%) _pd_proc_ls_prof_wR_expected 0.030 # 3.016(%) _refine_ls_R_I_factor 0.010 # 0.987(%) _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 84 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.141 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max <.001 _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 2.0 _pd_proc_2theta_range_max 45.0 _pd_proc_2theta_range_inc 0.005 _pd_proc_wavelength .700486 _pd_block_diffractogram_id C4H6BCrF5N2-profile # 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 ? # The following items are used to identify the programs used. _computing_data_collection SPEC _computing_cell_refinement TOPAS-Academic _computing_data_reduction TOPAS-Academic _computing_structure_solution 'EXPO and TOPAS-Academic' _computing_structure_refinement TOPAS-Academic _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. 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 Cr1 Cr 4 0 0 0 1 2.099(54) F2 F 4 0.5 0.56667(41) 0.25 1 2.23(14) F3 F 8 0.07620(26) 0.36056(40) 0.80476(54) 1 6.93(12) F4 F 8 0.04534(31) 0.78590(38) 0.10480(50) 1 6.93(12) B5 B 4 0.5 0.2122(14) 0.25 1 6.93(12) N6 N 8 0.16668 0.0531 0.92445 1 2.67(11) C7 C 8 0.240054 0.09432154 0.8571623 1 2.67(11) C8 C 8 0.3394828 0.1489632 0.764615 1 2.67(11) H8a H 8 0.375569 0.08675798 0.6736919 1 2.67(11) H8b H 8 0.3216876 0.2278865 0.6987844 1 2.67(11) H8c H 8 0.389852 0.1699776 0.8574607 1 2.67(11) # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol ? ? ? ? ? ? ? ? #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 C7 N6 1.06(3) 1_555 1_555 C7 C8 1.44(3) 1_555 1_555 C8 H8a 1.0(1) 1_555 1_555 C8 H8b 1.0(1) 1_555 1_555 C8 H8c 1.0(1) 1_555 1_555 C8 C7 1.44(3) 1_555 1_555 H8a C8 1.0(1) 1_555 1_555 H8b C8 1.0(1) 1_555 1_555 H8c C8 1.0(1) 1_555 1_555 B5 F3 1.30(5) 1_555 1_555 B5 F3 1.30(5) 1_555 2_556 B5 F4 1.37(5) 1_555 1_555 B5 F4 1.37(5) 1_555 2_556 N6 C7 1.06(3) 1_555 1_555 N6 Cr1 2.12(2) 1_555 1_555 F2 Cr1 1.94(2) 1_555 1_555 F2 Cr1 1.94(2) 1_555 2_556 F3 B5 1.30(5) 1_555 1_555 F4 B5 1.37(5) 1_555 1_555 Cr1 F2 1.94(2) 1_555 1_555 Cr1 F2 1.94(2) 1_555 3_557 Cr1 N6 2.12(2) 1_555 1_555 Cr1 N6 2.12(2) 1_555 3_557 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N6 C7 C8 179(4) 1_555 1_555 1_555 H8a C8 H8b 109.47 1_555 1_555 1_555 H8a C8 H8c 109.47 1_555 1_555 1_555 H8a C8 C7 109.48 1_555 1_555 1_555 H8b C8 H8c 109.47 1_555 1_555 1_555 H8b C8 C7 109.48 1_555 1_555 1_555 H8c C8 C7 109.47 1_555 1_555 1_555 F3 B5 F3 108.5(6) 1_555 1_555 2_556 F3 B5 F4 110(1) 1_555 1_555 1_555 F3 B5 F4 109.0(9) 1_555 1_555 2_556 F3 B5 F4 109.0(9) 2_556 1_555 1_555 F3 B5 F4 110(1) 2_556 1_555 2_556 F4 B5 F4 111.3(6) 1_555 1_555 2_556 C7 N6 Cr1 164(2) 1_555 1_555 1_555 Cr1 F2 Cr1 138(1) 1_555 1_555 2_556 F2 Cr1 F2 180.00 1_555 1_555 3_557 F2 Cr1 N6 87.8(3) 1_555 1_555 1_555 F2 Cr1 N6 92.2(3) 1_555 1_555 3_557 F2 Cr1 N6 92.2(3) 3_557 1_555 1_555 F2 Cr1 N6 87.8(3) 3_557 1_555 3_557 N6 Cr1 N6 179.97 1_555 1_555 3_557 #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./