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.
#==============================================================================

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