# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
S.Lapidus
A.C.McConnell
P.W.Stephens
J.S.Miller
_publ_contact_author_name        'Joel S. Miller'
_publ_contact_author_email       jsmiller@chem.utah.edu

data_ACM2001_glass
_database_code_depnum_ccdc_archive 'CCDC 806337'
#TrackingRef 'web_deposit_cif_file_0_SaulLapidus_1294115939.cif'

# 5. CHEMICAL DATA

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C6 I Mn N4 O'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C6 I Mn N4 O'
_chemical_formula_weight         325.94
_exptl_crystal_density_diffrn    2.23380

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_space_group_name_H-M_alt        Pnam

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+1/2, -y+1/2, -z+1/2'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, y, -z+1/2'
7 '-x+1/2, y+1/2, z+1/2'
8 'x+1/2, -y+1/2, z'

_cell_length_a                   12.71226(38)
_cell_length_b                   9.99610(30)
_cell_length_c                   7.62678(23)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     969.159(50)
_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    ? # include if applicable
_exptl_absorpt_correction_type   ? # 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     0.699942
_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        7101
_pd_meas_2theta_range_min        4.5
_pd_meas_2theta_range_max        40.0
_pd_meas_2theta_range_inc        0.005

# 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      
;
Molecules are defined as rigid bodies using the z-matrix function
implemented in TOPAS-Academic. The same isotropic displacement parameters are
assigned to all atoms within a molecule.
;

# 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  
;
1 Pearson-Voight peaks and Chebyshev polynomial with 7 coefficients
;
_pd_proc_ls_pref_orient_corr     
;
none
;

_pd_proc_ls_prof_R_factor        0.04999 # 4.999(%)
_pd_proc_ls_prof_wR_factor       0.06329 # 6.329(%)
_pd_proc_ls_prof_wR_expected     0.04909 # 4.909(%)
_refine_ls_R_I_factor            ?
_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_extinction_coef       ?
_refine_ls_number_parameters     42
_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   1.289

_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_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        4.5
_pd_proc_2theta_range_max        40.0
_pd_proc_2theta_range_inc        0.005
_pd_proc_wavelength              0.699942

_pd_block_diffractogram_id       ACM2001_glass
# 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    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

O1 O 4 0.32799(61) 0.50518(90) 0.25 1 1.22(24)
Mn1 Mn 4 0.23137(18) 0.69412(25) 0.25 1 1.723(72)
I1 I 4 0.11085(10) 0.93153(15) 0.25 1 4.128(47)
C1 C 4 0.53342 0.85027 0.75 1 1.50(13)
C2 C 4 0.43166 0.80557 0.75 1 1.50(13)
C3 C 8 0.37492 0.78065 0.59477 1 1.50(13)
C4 C 8 0.59015 0.87519 0.59477 1 1.50(13)
N1 N 8 0.33505 0.76314 0.46297 1 1.50(13)
N2 N 8 0.63006 0.89270 0.46297 1 1.50(13)

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;

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
_geom_bond_publ_flag
I1 Mn1 2.8248(28) . . yes
Mn1 O1 2.2529(91) . . yes
Mn1 N1 2.203(18) . . yes
Mn1 N1 2.203(18) . 6_555 yes
Mn1 N2 2.248(11) . 3_465 yes
Mn1 N2 2.248(11) . 8_465 yes
N1 C3 1.1393(64) . . yes
N2 C4 1.1393(64) . . yes
C1 C2 1.368(20) . . yes
C1 C4 1.4085(81) . . yes
C1 C4 1.4085(81) . 6_556 yes
C2 C3 1.4085(81) . . yes
C2 C3 1.4085(81) . 6_556 yes

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
_geom_angle_publ_flag
I1 Mn1 O1 179.81(21) . . . yes
I1 Mn1 N1 93.52(25) . . . yes
I1 Mn1 N2 90.77(53) . . 3_465 yes
I1 Mn1 N2 90.77(53) . . 8_465 yes
I1 Mn1 N1 93.52(25) . . 6_555 yes
O1 Mn1 N1 86.35(29) . . . yes
O1 Mn1 N2 89.36(55) . . 3_465 yes
O1 Mn1 N2 89.36(55) . . 8_465 yes
O1 Mn1 N1 86.35(29) . . 6_555 yes
N1 Mn1 N2 175.50(42) . . 3_465 yes
N1 Mn1 N2 86.0(13) . . 8_465 yes
N1 Mn1 N1 95.0(16) . . 6_555 yes
N2 Mn1 N2 92.6(11) 3_465 . 8_465 yes
N1 Mn1 N2 86.0(13) 6_555 . 3_465 yes
N1 Mn1 N2 175.50(42) 6_555 . 8_465 yes
Mn1 N1 C3 164.80(16) . . . yes
Mn1 N2 C4 146.44(19) 3_565 . . yes
C2 C1 C4 122.81(49) . . . yes
C2 C1 C4 122.81(49) . . 6_556 yes
C4 C1 C4 114.39(99) . . 6_556 yes
C1 C2 C3 122.81(49) . . . yes
C1 C2 C3 122.81(49) . . 6_556 yes
C3 C2 C3 114.39(99) . . 6_556 yes
N1 C3 C2 175.27(87) . . . yes
N2 C4 C1 175.27(87) . . . yes