# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_IMP-16Mn

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H61 Cl Mn4 N36 O4 Si2, 20(C3 H7 N O)'
_chemical_formula_sum            'C128 H201 Cl Mn4 N56 O24 Si2'
_chemical_formula_weight         3219.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/mnm

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y-1/2, -x-1/2, -z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y, -x, z'
'y, x, z'

_cell_length_a                   18.8266(5)
_cell_length_b                   18.8266(5)
_cell_length_c                   25.4638(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9025.4(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173
_cell_measurement_reflns_used    3726
_cell_measurement_theta_min      2.3449
_cell_measurement_theta_max      72.2041

_exptl_crystal_description       cubes
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3396
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16838
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         72.35
_reflns_number_total             4666
_reflns_number_gt                2075
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1563P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4666
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2943
_refine_ls_wR_factor_gt          0.2599
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.60140(5) 0.39860(5) 0.5000 0.0875(5) Uani 1 4 d S . .
Mn2 Mn 0.5000 0.5000 0.60784(7) 0.0896(5) Uani 1 4 d S . .
Cl1 Cl 0.5000 0.5000 0.5000 0.0855(8) Uani 1 8 d S . .
Si1 Si 0.5000 0.0000 0.7500 0.0886(7) Uani 1 4 d S . .
N1 N 0.5394(2) 0.34870(19) 0.56325(16) 0.0899(11) Uani 1 1 d . . .
N2 N 0.50375(19) 0.3828(2) 0.60060(17) 0.0924(11) Uani 1 1 d . . .
N3 N 0.4829(2) 0.3356(2) 0.63761(17) 0.0945(11) Uani 1 1 d . . .
C4 C 0.5075(2) 0.2734(2) 0.6189(2) 0.0895(13) Uani 1 1 d . . .
N5 N 0.5421(2) 0.2796(2) 0.57498(18) 0.0953(11) Uani 1 1 d . . .
C6 C 0.5009(2) 0.2072(2) 0.6495(2) 0.0911(13) Uani 1 1 d . . .
C7 C 0.4620(3) 0.2041(3) 0.6953(2) 0.1153(18) Uani 1 1 d . . .
H7A H 0.4370 0.2448 0.7073 0.138 Uiso 1 1 calc R . .
C8 C 0.4596(3) 0.1411(3) 0.7237(2) 0.1171(18) Uani 1 1 d . . .
H8A H 0.4317 0.1391 0.7548 0.140 Uiso 1 1 calc R . .
C9 C 0.4969(2) 0.0810(2) 0.7081(2) 0.0886(12) Uani 1 1 d . . .
C10 C 0.5349(3) 0.0858(3) 0.6617(2) 0.1085(16) Uani 1 1 d . . .
H10A H 0.5595 0.0450 0.6495 0.130 Uiso 1 1 calc R . .
C11 C 0.5384(3) 0.1477(2) 0.6326(2) 0.1102(17) Uani 1 1 d . . .
H11A H 0.5661 0.1496 0.6014 0.132 Uiso 1 1 calc R . .
O20 O 0.6811(3) 0.3189(3) 0.5000 0.126(2) Uani 1 4 d S . .
O30 O 0.5000 0.5000 0.6925(3) 0.129(3) Uani 1 4 d S . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O20 2.123(7) . ?
Mn1 N1 2.199(4) 15_665 ?
Mn1 N1 2.199(4) 10_556 ?
Mn1 N1 2.199(4) 8_666 ?
Mn1 N1 2.199(4) . ?
Mn1 Cl1 2.6998(14) . ?
Mn2 O30 2.157(9) . ?
Mn2 N2 2.214(4) . ?
Mn2 N2 2.214(4) 16 ?
Mn2 N2 2.214(4) 15_665 ?
Mn2 N2 2.214(4) 2_665 ?
Mn2 Cl1 2.7459(17) . ?
Cl1 Mn1 2.6998(14) 9_666 ?
Cl1 Mn2 2.7459(17) 9_666 ?
Si1 C9 1.862(5) . ?
Si1 C9 1.862(5) 11_667 ?
Si1 C9 1.862(5) 2_655 ?
Si1 C9 1.862(5) 12_657 ?
N1 N2 1.330(5) . ?
N1 N5 1.336(5) . ?
N2 N3 1.354(5) . ?
N3 C4 1.345(6) . ?
C4 N5 1.300(6) . ?
C4 C6 1.475(6) . ?
C6 C7 1.378(7) . ?
C6 C11 1.393(6) . ?
C7 C8 1.390(7) . ?
C8 C9 1.391(6) . ?
C9 C10 1.383(7) . ?
C10 C11 1.383(7) . ?

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_3
_geom_angle_publ_flag
O20 Mn1 N1 94.19(10) . 15_665 ?
O20 Mn1 N1 94.19(10) . 10_556 ?
N1 Mn1 N1 171.6(2) 15_665 10_556 ?
O20 Mn1 N1 94.19(10) . 8_666 ?
N1 Mn1 N1 94.2(2) 15_665 8_666 ?
N1 Mn1 N1 85.2(2) 10_556 8_666 ?
O20 Mn1 N1 94.19(10) . . ?
N1 Mn1 N1 85.2(2) 15_665 . ?
N1 Mn1 N1 94.2(2) 10_556 . ?
N1 Mn1 N1 171.6(2) 8_666 . ?
O20 Mn1 Cl1 180.00(7) . . ?
N1 Mn1 Cl1 85.81(10) 15_665 . ?
N1 Mn1 Cl1 85.81(10) 10_556 . ?
N1 Mn1 Cl1 85.81(10) 8_666 . ?
N1 Mn1 Cl1 85.81(10) . . ?
O30 Mn2 N2 94.77(12) . . ?
O30 Mn2 N2 94.77(12) . 16 ?
N2 Mn2 N2 93.25(19) . 16 ?
O30 Mn2 N2 94.77(12) . 15_665 ?
N2 Mn2 N2 85.96(19) . 15_665 ?
N2 Mn2 N2 170.5(2) 16 15_665 ?
O30 Mn2 N2 94.77(12) . 2_665 ?
N2 Mn2 N2 170.5(2) . 2_665 ?
N2 Mn2 N2 85.96(19) 16 2_665 ?
N2 Mn2 N2 93.25(19) 15_665 2_665 ?
O30 Mn2 Cl1 180.000(1) . . ?
N2 Mn2 Cl1 85.23(12) . . ?
N2 Mn2 Cl1 85.23(12) 16 . ?
N2 Mn2 Cl1 85.23(12) 15_665 . ?
N2 Mn2 Cl1 85.23(12) 2_665 . ?
Mn1 Cl1 Mn1 180.0 . 9_666 ?
Mn1 Cl1 Mn2 90.0 . 9_666 ?
Mn1 Cl1 Mn2 90.0 9_666 9_666 ?
Mn1 Cl1 Mn2 90.0 . . ?
Mn1 Cl1 Mn2 90.0 9_666 . ?
Mn2 Cl1 Mn2 180.0 9_666 . ?
C9 Si1 C9 109.19(15) . 11_667 ?
C9 Si1 C9 110.0(3) . 2_655 ?
C9 Si1 C9 109.19(15) 11_667 2_655 ?
C9 Si1 C9 109.19(15) . 12_657 ?
C9 Si1 C9 110.0(3) 11_667 12_657 ?
C9 Si1 C9 109.19(15) 2_655 12_657 ?
N2 N1 N5 109.2(4) . . ?
N2 N1 Mn1 125.8(3) . . ?
N5 N1 Mn1 124.1(3) . . ?
N1 N2 N3 109.1(4) . . ?
N1 N2 Mn2 123.8(3) . . ?
N3 N2 Mn2 125.9(3) . . ?
C4 N3 N2 103.0(4) . . ?
N5 C4 N3 113.5(4) . . ?
N5 C4 C6 124.8(4) . . ?
N3 C4 C6 121.3(5) . . ?
C4 N5 N1 105.1(4) . . ?
C7 C6 C11 119.8(5) . . ?
C7 C6 C4 121.8(4) . . ?
C11 C6 C4 118.3(5) . . ?
C6 C7 C8 119.6(5) . . ?
C7 C8 C9 121.9(5) . . ?
C10 C9 C8 116.9(5) . . ?
C10 C9 Si1 121.8(3) . . ?
C8 C9 Si1 121.2(4) . . ?
C9 C10 C11 122.5(5) . . ?
C10 C11 C6 119.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        72.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.054

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.009 -0.002 0.325 6569 1830 ' '
_platon_squeeze_details          
;
 Due to the severe disorder across symmetry, only the oxygen atoms of the
 coordinated solvent molecules could be reliably located. From the looks
 of the electron density maps, combined with the solvent list given by the
 chemist, the most likely solvent is dmf (C3H7NO).
 So, at the time of running SQUEEZE, the asu contents were low by
 0.5(C3H7N). However, SQUEEZE does not remove electron denisty that is
 within bonding distance of defined atoms, so the contribution of the
 carbonyl carbon would not be removed, meaning that 0.5(C2H7N) = 13 e/asu
 of that removed by SQUEEZE would be due to the coordinated solvent.
 
 SQUEEZE suggested 1830 e/cell = 114.4 e/asu.
 As detailed above, the disorder of the coordinated solvent accounts for
 13 e/asu of this, leaving 101.4 e/asu for the included solvent.
 The included solvent is presumed to be dmf (C3H7NO) = 40e.
 2.5dmf = 100e so this was used as the solvent present.
 2.5dmf per asu = 20dmf per Mn4 unit.
 
 So, atom list low by 0.125(H) + 0.5(C3H7N) 2.5(C3H7NO)
 = H0.125+(C1.5 H3.5 N0.5)+(C7.5 H17.5 N2.5 O2.5)
 = C9 H21.125 N3 O2.5, and UNIT low by C144 H338 N48 O40,
 i.e. C112 H64 N64 O8 Cl2 Mn8 Si4
;
_database_code_depnum_ccdc_archive 'CCDC 989922'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_IMP-17Mn

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H44 Mn2 N20 O4 Si, 28(C3 H7 N O)'
_chemical_formula_sum            'C124 H240 Mn2 N48 O32 Si'
_chemical_formula_weight         3053.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   36.7051(15)
_cell_length_b                   36.7051(15)
_cell_length_c                   36.7051(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     49452(6)
_cell_formula_units_Z            24
_cell_measurement_temperature    173
_cell_measurement_reflns_used    1345
_cell_measurement_theta_min      1.7007
_cell_measurement_theta_max      72.0927

_exptl_crystal_description       blocks
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_F_000             39360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    3.956
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_reflns_number            16079
_diffrn_reflns_av_unetI/netI     0.1605
_diffrn_reflns_av_R_equivalents  0.2211
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.949
_diffrn_reflns_theta_max         72.240
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4003
_reflns_number_gt                786
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1108P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4003
_refine_ls_number_parameters     116
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2798
_refine_ls_R_factor_gt           0.1447
_refine_ls_wR_factor_ref         0.4057
_refine_ls_wR_factor_gt          0.3462
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.906
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.5000 0.5000 0.1417(13) Uani 1 6 d S T P . .
Mn2 Mn 0.56378(5) 0.56378(5) 0.56378(5) 0.1715(13) Uani 1 3 d S T P . .
Si1 Si 0.7500 0.3750 0.5000 0.1465(17) Uani 1 4 d S T P . .
N1 N 0.5578(2) 0.4907(3) 0.5117(2) 0.146(3) Uani 1 1 d . . . . .
N2 N 0.5794(3) 0.5125(3) 0.5335(3) 0.159(3) Uani 1 1 d . . . . .
N3 N 0.6138(2) 0.5000(3) 0.5363(2) 0.145(2) Uani 1 1 d . . . . .
C4 C 0.6115(4) 0.4698(3) 0.5152(3) 0.154(4) Uani 1 1 d . . . . .
N5 N 0.5782(3) 0.4636(2) 0.4997(3) 0.155(3) Uani 1 1 d . . . . .
C6 C 0.6461(3) 0.4462(3) 0.5105(3) 0.180(5) Uani 1 1 d . . . . .
C7 C 0.6790(4) 0.4525(3) 0.5342(4) 0.208(6) Uani 1 1 d . . . . .
H7A H 0.6799 0.4713 0.5519 0.250 Uiso 1 1 calc R U . . .
C8 C 0.7074(3) 0.4291(5) 0.5283(4) 0.187(5) Uani 1 1 d . . . . .
H8A H 0.7284 0.4313 0.5431 0.224 Uiso 1 1 calc R U . . .
C9 C 0.7069(4) 0.4022(3) 0.5018(3) 0.159(4) Uani 1 1 d . . . . .
C10 C 0.6763(3) 0.4018(3) 0.4798(3) 0.161(4) Uani 1 1 d . . . . .
H10A H 0.6761 0.3848 0.4603 0.193 Uiso 1 1 calc R U . . .
C11 C 0.6478(3) 0.4226(3) 0.4834(3) 0.160(4) Uani 1 1 d . . . . .
H11A H 0.6283 0.4208 0.4666 0.192 Uiso 1 1 calc R U . . .
O20 O 0.5935(3) 0.5457(2) 0.6111(2) 0.234(4) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N1 2.193(9) 57_666 ?
Mn1 N1 2.193(9) 9 ?
Mn1 N1 2.193(9) 53_666 ?
Mn1 N1 2.193(9) 5 ?
Mn1 N1 2.193(9) 49_666 ?
Mn1 N1 2.193(9) . ?
Mn2 O20 2.154(10) 9 ?
Mn2 O20 2.154(10) 5 ?
Mn2 O20 2.154(10) . ?
Mn2 N2 2.261(10) . ?
Mn2 N2 2.261(10) 9 ?
Mn2 N2 2.261(10) 5 ?
Si1 C9 1.872(13) 69_765 ?
Si1 C9 1.872(13) 27_645 ?
Si1 C9 1.872(13) 95_566 ?
Si1 C9 1.872(13) . ?
N1 N5 1.320(10) . ?
N1 N2 1.379(12) . ?
N2 N3 1.349(10) . ?
N3 C4 1.353(12) . ?
C4 N5 1.368(14) . ?
C4 C6 1.551(15) . ?
C6 C11 1.319(15) . ?
C6 C7 1.504(17) . ?
C7 C8 1.368(16) . ?
C8 C9 1.384(15) . ?
C9 C10 1.382(14) . ?
C10 C11 1.303(12) . ?

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_3
_geom_angle_publ_flag
N1 Mn1 N1 180.0 57_666 9 ?
N1 Mn1 N1 89.5(4) 57_666 53_666 ?
N1 Mn1 N1 90.5(4) 9 53_666 ?
N1 Mn1 N1 90.5(4) 57_666 5 ?
N1 Mn1 N1 89.5(4) 9 5 ?
N1 Mn1 N1 180.0(5) 53_666 5 ?
N1 Mn1 N1 89.5(4) 57_666 49_666 ?
N1 Mn1 N1 90.5(4) 9 49_666 ?
N1 Mn1 N1 89.5(4) 53_666 49_666 ?
N1 Mn1 N1 90.5(4) 5 49_666 ?
N1 Mn1 N1 90.5(4) 57_666 . ?
N1 Mn1 N1 89.5(4) 9 . ?
N1 Mn1 N1 90.4(4) 53_666 . ?
N1 Mn1 N1 89.6(4) 5 . ?
N1 Mn1 N1 180.0(5) 49_666 . ?
O20 Mn2 O20 89.8(3) 9 5 ?
O20 Mn2 O20 89.8(3) 9 . ?
O20 Mn2 O20 89.8(3) 5 . ?
O20 Mn2 N2 176.4(4) 9 . ?
O20 Mn2 N2 93.7(4) 5 . ?
O20 Mn2 N2 90.7(4) . . ?
O20 Mn2 N2 90.7(4) 9 9 ?
O20 Mn2 N2 176.4(4) 5 9 ?
O20 Mn2 N2 93.7(4) . 9 ?
N2 Mn2 N2 85.7(5) . 9 ?
O20 Mn2 N2 93.7(4) 9 5 ?
O20 Mn2 N2 90.7(4) 5 5 ?
O20 Mn2 N2 176.4(4) . 5 ?
N2 Mn2 N2 85.7(5) . 5 ?
N2 Mn2 N2 85.7(5) 9 5 ?
C9 Si1 C9 106.5(3) 69_765 27_645 ?
C9 Si1 C9 115.6(6) 69_765 95_566 ?
C9 Si1 C9 106.5(3) 27_645 95_566 ?
C9 Si1 C9 106.5(3) 69_765 . ?
C9 Si1 C9 115.6(6) 27_645 . ?
C9 Si1 C9 106.5(3) 95_566 . ?
N5 N1 N2 107.9(8) . . ?
N5 N1 Mn1 126.8(10) . . ?
N2 N1 Mn1 125.3(7) . . ?
N3 N2 N1 112.6(8) . . ?
N3 N2 Mn2 118.9(10) . . ?
N1 N2 Mn2 128.5(7) . . ?
N2 N3 C4 100.0(10) . . ?
N3 C4 N5 115.7(12) . . ?
N3 C4 C6 117.9(15) . . ?
N5 C4 C6 126.4(12) . . ?
N1 N5 C4 103.8(9) . . ?
C11 C6 C7 120.0(9) . . ?
C11 C6 C4 119.3(12) . . ?
C7 C6 C4 120.5(13) . . ?
C8 C7 C6 114.9(12) . . ?
C7 C8 C9 123.3(11) . . ?
C10 C9 C8 115.3(11) . . ?
C10 C9 Si1 131.2(9) . . ?
C8 C9 Si1 113.2(11) . . ?
C11 C10 C9 125.9(11) . . ?
C10 C11 C6 119.9(11) . . ?

_refine_diff_density_max         0.381
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.076

_shelxl_version_number           2013-4

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.241 0.021 -0.007 34224 29377 ' '
_platon_squeeze_details          
;
 On the basis of the solvents used, and by analogy with the structure of
 the isomorphous Cd analogue (RD1109b), both the coordinated and included
 solvents were assumed to be dmf (C3H7NO) = 40e.
 Due to severe disorder, only the oxygen atom of the coordinated solvent
 molecule could be reliably located.
 So, at the time of running SQUEEZE, the asu contents were low by
 (C3H7N). However, SQUEEZE does not remove electron density that is
 within bonding distance of defined atoms, so the contribution of the
 carbonyl carbon would not be removed, meaning that (C2H7N) = 26 e/asu
 of that removed by SQUEEZE would be due to the coordinated solvent.
 
 SQUEEZE suggested 29377 e/cell = 306 e/asu.
 As detailed above, the disorder of the coordinated solvent accounts for
 26 e/asu of this, leaving 280 e/asu for the included solvent.
 The included solvent is presumed to be dmf (C3H7NO) = 40e.
 7dmf = 280e so this was used as the solvent present.
 7dmf per asu = 28dmf per LMn2 unit.

 So, atom list low by (C3H7N) + 7(C3H7NO) = C24 H56 N8 O7,
 and UNIT low by C2304 H5376 N768 O672,
 i.e. C672 H384 N384 O96 Si24 Mn48
;
_database_code_depnum_ccdc_archive 'CCDC 989923'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_IMP-17Cd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H44 Cd2 N20 O4 Si, 16(C3 H7 N O)'
_chemical_formula_sum            'C88 H156 Cd2 N36 O20 Si'
_chemical_formula_weight         2291.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Ia-3d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   36.97447(15)
_cell_length_b                   36.97447(15)
_cell_length_c                   36.97447(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     50548.2(4)
_cell_formula_units_Z            24
_cell_measurement_temperature    173
_cell_measurement_reflns_used    51071
_cell_measurement_theta_min      1.6883
_cell_measurement_theta_max      72.2512

_exptl_crystal_description       blocks
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             28944
_exptl_absorpt_coefficient_mu    5.047
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            161857
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         72.40
_reflns_number_total             4182
_reflns_number_gt                3535
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0523P)²+127.0912P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4182
_refine_ls_number_parameters     172
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.5000 0.5000 0.5000 0.05011(17) Uani 1 6 d S . .
Cd2 Cd 0.564168(8) 0.564168(8) 0.564168(8) 0.06408(17) Uani 1 3 d S A .
Si1 Si 0.7500 0.3750 0.5000 0.0490(4) Uani 1 4 d S . .
N1 N 0.56234(8) 0.49157(8) 0.51229(8) 0.0606(7) Uani 1 1 d . . .
N2 N 0.58150(8) 0.51247(9) 0.53423(8) 0.0610(7) Uani 1 1 d . . .
N3 N 0.61507(8) 0.49952(9) 0.53745(9) 0.0640(7) Uani 1 1 d . . .
C4 C 0.61505(10) 0.47014(10) 0.51643(10) 0.0587(8) Uani 1 1 d . . .
N5 N 0.58281(8) 0.46441(8) 0.50036(8) 0.0576(7) Uani 1 1 d . . .
C6 C 0.64702(9) 0.44739(10) 0.51172(9) 0.0574(8) Uani 1 1 d . . .
C7 C 0.67505(11) 0.44887(12) 0.53698(11) 0.0710(10) Uani 1 1 d . . .
H7A H 0.6733 0.4646 0.5573 0.085 Uiso 1 1 calc R . .
C8 C 0.70512(10) 0.42772(11) 0.53254(11) 0.0683(10) Uani 1 1 d . . .
H8A H 0.7241 0.4293 0.5498 0.082 Uiso 1 1 calc R . .
C9 C 0.70878(9) 0.40415(9) 0.50377(8) 0.0524(7) Uani 1 1 d . . .
C10 C 0.68050(9) 0.40284(11) 0.47911(9) 0.0616(9) Uani 1 1 d . . .
H10A H 0.6822 0.3870 0.4590 0.074 Uiso 1 1 calc R . .
C11 C 0.65001(10) 0.42394(10) 0.48308(10) 0.0616(9) Uani 1 1 d . . .
H11A H 0.6310 0.4222 0.4659 0.074 Uiso 1 1 calc R . .
O20 O 0.59518(12) 0.54615(12) 0.61405(10) 0.1088(12) Uani 1 1 d D . .
C20 C 0.6278(3) 0.5376(5) 0.6090(4) 0.138(4) Uani 0.633(15) 1 d PDU A 1
H20A H 0.6391 0.5456 0.5874 0.165 Uiso 0.633(15) 1 calc PR A 1
N21 N 0.6473(3) 0.5180(4) 0.6322(4) 0.184(5) Uani 0.633(15) 1 d PDU A 1
C22 C 0.6284(5) 0.4973(6) 0.6602(5) 0.206(7) Uani 0.633(15) 1 d PDU A 1
H22A H 0.6025 0.4963 0.6545 0.309 Uiso 0.633(15) 1 calc PR A 1
H22B H 0.6318 0.5092 0.6837 0.309 Uiso 0.633(15) 1 calc PR A 1
H22C H 0.6383 0.4728 0.6612 0.309 Uiso 0.633(15) 1 calc PR A 1
C23 C 0.6853(4) 0.5109(6) 0.6269(5) 0.247(11) Uani 0.633(15) 1 d PDU A 1
H23A H 0.6947 0.5267 0.6078 0.371 Uiso 0.633(15) 1 calc PR A 1
H23B H 0.6887 0.4856 0.6199 0.371 Uiso 0.633(15) 1 calc PR A 1
H23C H 0.6984 0.5156 0.6495 0.371 Uiso 0.633(15) 1 calc PR A 1
C20' C 0.6241(6) 0.5304(11) 0.6190(9) 0.170(9) Uiso 0.367(15) 1 d PDU A 2
H20B H 0.6429 0.5338 0.6019 0.204 Uiso 0.367(15) 1 calc PR A 2
N21' N 0.6304(8) 0.5087(9) 0.6471(8) 0.204(7) Uiso 0.367(15) 1 d PDU A 2
C22' C 0.6035(9) 0.5039(10) 0.6752(9) 0.250(19) Uiso 0.367(15) 1 d PD A 2
H22D H 0.6157 0.4986 0.6982 0.375 Uiso 0.367(15) 1 d PR A 2
H22E H 0.5874 0.4839 0.6690 0.375 Uiso 0.367(15) 1 d PR A 2
H22F H 0.5893 0.5262 0.6777 0.375 Uiso 0.367(15) 1 d PR A 2
C23' C 0.6594(8) 0.4824(7) 0.6440(8) 0.192(13) Uiso 0.367(15) 1 d PD A 2
H23D H 0.6496 0.4594 0.6351 0.288 Uiso 0.367(15) 1 calc PR A 2
H23E H 0.6705 0.4786 0.6678 0.288 Uiso 0.367(15) 1 calc PR A 2
H23F H 0.6777 0.4913 0.6270 0.288 Uiso 0.367(15) 1 calc PR A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.370(3) 9 ?
Cd1 N1 2.370(3) . ?
Cd1 N1 2.370(3) 53_666 ?
Cd1 N1 2.370(3) 49_666 ?
Cd1 N1 2.370(3) 5 ?
Cd1 N1 2.370(3) 57_666 ?
Cd2 O20 2.272(4) 9 ?
Cd2 O20 2.272(4) 5 ?
Cd2 O20 2.272(4) . ?
Cd2 N2 2.300(3) 9 ?
Cd2 N2 2.300(3) . ?
Cd2 N2 2.300(3) 5 ?
Si1 C9 1.872(3) 27_645 ?
Si1 C9 1.872(3) 95_566 ?
Si1 C9 1.872(3) 69_765 ?
Si1 C9 1.872(3) . ?
N1 N2 1.325(4) . ?
N1 N5 1.332(4) . ?
N2 N3 1.336(4) . ?
N3 C4 1.336(5) . ?
C4 N5 1.349(5) . ?
C4 C6 1.461(5) . ?
C6 C11 1.373(5) . ?
C6 C7 1.396(5) . ?
C7 C8 1.369(5) . ?
C8 C9 1.382(5) . ?
C9 C10 1.388(5) . ?
C10 C11 1.379(5) . ?
O20 C20' 1.232(10) . ?
O20 C20 1.259(8) . ?
C20 N21 1.335(8) . ?
N21 C23 1.445(9) . ?
N21 C22 1.464(9) . ?
C20' N21' 1.331(9) . ?
N21' C22' 1.451(9) . ?
N21' C23' 1.453(10) . ?

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_3
_geom_angle_publ_flag
N1 Cd1 N1 88.08(11) 9 . ?
N1 Cd1 N1 91.92(11) 9 53_666 ?
N1 Cd1 N1 91.92(11) . 53_666 ?
N1 Cd1 N1 91.92(11) 9 49_666 ?
N1 Cd1 N1 180.000(1) . 49_666 ?
N1 Cd1 N1 88.08(11) 53_666 49_666 ?
N1 Cd1 N1 88.08(11) 9 5 ?
N1 Cd1 N1 88.08(11) . 5 ?
N1 Cd1 N1 180.0 53_666 5 ?
N1 Cd1 N1 91.92(11) 49_666 5 ?
N1 Cd1 N1 180.00(3) 9 57_666 ?
N1 Cd1 N1 91.92(11) . 57_666 ?
N1 Cd1 N1 88.08(11) 53_666 57_666 ?
N1 Cd1 N1 88.08(11) 49_666 57_666 ?
N1 Cd1 N1 91.92(11) 5 57_666 ?
O20 Cd2 O20 88.64(16) 9 5 ?
O20 Cd2 O20 88.64(16) 9 . ?
O20 Cd2 O20 88.64(16) 5 . ?
O20 Cd2 N2 90.37(13) 9 9 ?
O20 Cd2 N2 178.07(14) 5 9 ?
O20 Cd2 N2 92.99(13) . 9 ?
O20 Cd2 N2 178.07(14) 9 . ?
O20 Cd2 N2 92.99(13) 5 . ?
O20 Cd2 N2 90.37(13) . . ?
N2 Cd2 N2 88.03(11) 9 . ?
O20 Cd2 N2 92.99(13) 9 5 ?
O20 Cd2 N2 90.37(13) 5 5 ?
O20 Cd2 N2 178.07(14) . 5 ?
N2 Cd2 N2 88.03(11) 9 5 ?
N2 Cd2 N2 88.03(11) . 5 ?
C9 Si1 C9 109.37(10) 27_645 95_566 ?
C9 Si1 C9 109.37(10) 27_645 69_765 ?
C9 Si1 C9 109.7(2) 95_566 69_765 ?
C9 Si1 C9 109.7(2) 27_645 . ?
C9 Si1 C9 109.37(10) 95_566 . ?
C9 Si1 C9 109.37(10) 69_765 . ?
N2 N1 N5 109.8(3) . . ?
N2 N1 Cd1 124.1(2) . . ?
N5 N1 Cd1 126.0(2) . . ?
N1 N2 N3 110.0(3) . . ?
N1 N2 Cd2 129.1(2) . . ?
N3 N2 Cd2 120.9(2) . . ?
C4 N3 N2 103.8(3) . . ?
N3 C4 N5 112.6(3) . . ?
N3 C4 C6 122.5(3) . . ?
N5 C4 C6 124.9(3) . . ?
N1 N5 C4 103.7(3) . . ?
C11 C6 C7 118.7(3) . . ?
C11 C6 C4 121.4(3) . . ?
C7 C6 C4 119.9(3) . . ?
C8 C7 C6 120.0(4) . . ?
C7 C8 C9 122.1(3) . . ?
C8 C9 C10 117.0(3) . . ?
C8 C9 Si1 120.0(3) . . ?
C10 C9 Si1 123.0(3) . . ?
C11 C10 C9 121.7(3) . . ?
C6 C11 C10 120.4(3) . . ?
C20' O20 Cd2 134.3(16) . . ?
C20 O20 Cd2 115.9(6) . . ?
O20 C20 N21 123.9(10) . . ?
C20 N21 C23 122.6(11) . . ?
C20 N21 C22 118.7(10) . . ?
C23 N21 C22 117.7(10) . . ?
O20 C20' N21' 123.7(16) . . ?
C20' N21' C22' 120.8(14) . . ?
C20' N21' C23' 118.1(15) . . ?
C22' N21' C23' 118.8(14) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        72.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.059

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.231 -0.006 -0.018 24477 15018 ' '
2 0.125 0.125 0.125 20 4 ' '
3 0.625 0.125 0.375 20 3 ' '
4 0.875 0.125 0.625 20 2 ' '
5 0.375 0.125 0.875 20 2 ' '
6 0.875 0.375 0.125 20 3 ' '
7 0.375 0.375 0.375 20 2 ' '
8 0.125 0.375 0.625 20 3 ' '
9 0.625 0.375 0.875 20 4 ' '
10 0.375 0.625 0.125 20 2 ' '
11 0.875 0.625 0.375 20 2 ' '
12 0.625 0.625 0.625 20 4 ' '
13 0.125 0.625 0.875 20 3 ' '
14 0.625 0.875 0.125 20 3 ' '
15 0.125 0.875 0.375 20 4 ' '
16 0.375 0.875 0.625 20 3 ' '
17 0.875 0.875 0.875 20 2 ' '
_platon_squeeze_details          
;
 SQUEEZE suggested 15066 e/cell = 156.9 e/asu.
 Before SQUEEZE, the solvent looked like dmf (C3H7NO) = 40e.
 4dmf = 160e so this was used as the solvent present.
 4dmf per asu = 16dmf per LCd2 moiety
 
 So, atom list low by 4(C3H7NO) = C12 H28 N4 O4,
 and UNIT low by C1152 H2688 N384 O384,
 i.e. C960 H1056 N480 O96 Si24 Cd48
;
_database_code_depnum_ccdc_archive 'CCDC 989924'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_IMP-17Cu

_audit_creation_method           SHELXL-2013

#Dr. Robert Davies
#Refcode:- LINMOF1

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H16 Cu2 N16 O4 Si'
_chemical_formula_sum            'C28 H16 Cu2 N16 O4 Si'
_chemical_formula_weight         795.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'z, x, y'
'-x+1/4, z+3/4, y+1/4'
'-z+1/2, -x, y+1/2'
'x+1/4, -z+1/4, y+3/4'
'z, -x, -y+1/2'
'x+1/4, z+3/4, -y+3/4'
'-z+1/2, x, -y'
'-x+1/4, -z+1/4, -y+1/4'
'y, z, x'
'y+1/2, -z+1/2, -x'
'z+3/4, y+1/4, -x+1/4'
'-y, z+1/2, -x+1/2'
'-z+1/4, -y+1/4, -x+1/4'
'-y+1/2, -z, x+1/2'
'z+3/4, -y+3/4, x+1/4'
'-z+3/4, y+1/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'z+1/2, x+1/2, y+1/2'
'-x+3/4, z+5/4, y+3/4'
'-z+1, -x+1/2, y+1'
'x+3/4, -z+3/4, y+5/4'
'z+1/2, -x+1/2, -y+1'
'x+3/4, z+5/4, -y+5/4'
'-z+1, x+1/2, -y+1/2'
'-x+3/4, -z+3/4, -y+3/4'
'y+1/2, z+1/2, x+1/2'
'y+1, -z+1, -x+1/2'
'z+5/4, y+3/4, -x+3/4'
'-y+1/2, z+1, -x+1'
'-z+3/4, -y+3/4, -x+3/4'
'-y+1, -z+1/2, x+1'
'z+5/4, -y+5/4, x+3/4'
'-z+5/4, y+3/4, x+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-z, -x, -y'
'x-1/4, -z-3/4, -y-1/4'
'z-1/2, x, -y-1/2'
'-x-1/4, z-1/4, -y-3/4'
'-z, x, y-1/2'
'-x-1/4, -z-3/4, y-3/4'
'z-1/2, -x, y'
'x-1/4, z-1/4, y-1/4'
'-y, -z, -x'
'-y-1/2, z-1/2, x'
'-z-3/4, -y-1/4, x-1/4'
'y, -z-1/2, x-1/2'
'z-1/4, y-1/4, x-1/4'
'y-1/2, z, -x-1/2'
'-z-3/4, y-3/4, -x-1/4'
'z-3/4, -y-1/4, -x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-z+1/2, -x+1/2, -y+1/2'
'x+1/4, -z-1/4, -y+1/4'
'z, x+1/2, -y'
'-x+1/4, z+1/4, -y-1/4'
'-z+1/2, x+1/2, y'
'-x+1/4, -z-1/4, y-1/4'
'z, -x+1/2, y+1/2'
'x+1/4, z+1/4, y+1/4'
'-y+1/2, -z+1/2, -x+1/2'
'-y, z, x+1/2'
'-z-1/4, -y+1/4, x+1/4'
'y+1/2, -z, x'
'z+1/4, y+1/4, x+1/4'
'y, z+1/2, -x'
'-z-1/4, y-1/4, -x+1/4'
'z-1/4, -y+1/4, -x-1/4'

_cell_length_a                   36.1906(18)
_cell_length_b                   36.1906(18)
_cell_length_c                   36.1906(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     47401(7)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24279
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            blue-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.669
_exptl_crystal_F_000             9600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.580
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_process_details   
;
Rigaku CrystalClear-SM Expert 3.1 b24
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_reflns_number            126009
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.083
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             3498
_reflns_number_gt                1134
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
Rigaku CrystalClear-SM Expert 3.1 b24
;
_computing_cell_refinement       
;
Rigaku CrystalClear-SM Expert 3.1 b24
;
_computing_data_reduction        
;
Rigaku CrystalClear-SM Expert 3.1 b24
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3498
_refine_ls_number_parameters     104
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.2228
_refine_ls_R_factor_gt           0.1359
_refine_ls_wR_factor_ref         0.4402
_refine_ls_wR_factor_gt          0.3710
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.94043(3) 0.44043(3) 0.05957(3) 0.2264(13) Uani 1 3 d S TU P . .
Cu2 Cu 1.0000 0.5000 0.0000 0.1917(13) Uani 1 6 d S TU P . .
O1 O 0.9086(3) 0.4503(3) 0.1056(3) 0.392(5) Uani 1 1 d . U . . .
C1 C 1.0296(3) 0.4860(3) 0.1132(3) 0.207(3) Uani 1 1 d . U . . .
C2 C 1.05218(19) 0.49005(18) 0.14564(17) 0.218(3) Uani 1 1 d G U . . .
C3 C 1.04404(17) 0.46952(17) 0.1771(2) 0.297(6) Uani 1 1 d G U . . .
H3 H 1.0237 0.4530 0.1770 0.356 Uiso 1 1 calc R U . . .
C4 C 1.0657(2) 0.47321(19) 0.20856(17) 0.291(5) Uani 1 1 d G U . . .
H4 H 1.0601 0.4592 0.2300 0.349 Uiso 1 1 calc R U . . .
C5 C 1.09553(19) 0.49742(19) 0.20863(17) 0.228(3) Uani 1 1 d G U . . .
C6 C 1.10367(15) 0.51795(15) 0.1772(2) 0.231(4) Uani 1 1 d G U . . .
H6 H 1.1240 0.5345 0.1773 0.278 Uiso 1 1 calc R U . . .
C7 C 1.0820(2) 0.51426(15) 0.14571(17) 0.222(3) Uani 1 1 d G U . . .
H7 H 1.0876 0.5283 0.1242 0.266 Uiso 1 1 calc R U . . .
N1 N 0.9859(3) 0.4667(2) 0.0776(3) 0.230(3) Uani 1 1 d . U . . .
N2 N 1.0081(3) 0.4893(2) 0.0585(2) 0.213(3) Uani 1 1 d . U . . .
N3 N 1.0355(2) 0.5006(2) 0.0798(2) 0.208(2) Uani 1 1 d . U . . .
N4 N 0.9993(3) 0.4653(2) 0.1128(2) 0.228(3) Uani 1 1 d . U . . .
Si1 Si 1.1250 0.5000 0.2500 0.230(2) Uani 1 4 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.008(9) 18_556 ?
Cu1 N1 2.008(9) 39_545 ?
Cu1 N1 2.008(9) . ?
Cu1 O1 2.056(9) 18_556 ?
Cu1 O1 2.056(9) 39_545 ?
Cu1 O1 2.056(9) . ?
Cu2 N2 2.172(9) . ?
Cu2 N2 2.172(9) 66_764 ?
Cu2 N2 2.172(9) 18_556 ?
Cu2 N2 2.172(9) 49_765 ?
Cu2 N2 2.172(9) 87_664 ?
Cu2 N2 2.172(9) 39_545 ?
C1 N4 1.329(11) . ?
C1 N3 1.337(11) . ?
C1 C2 1.438(11) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 Si1 1.841(6) . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
N1 N2 1.340(9) . ?
N1 N4 1.365(9) . ?
N2 N3 1.320(8) . ?
Si1 C5 1.841(10) 86_765 ?
Si1 C5 1.841(9) 5_565 ?
Si1 C5 1.841(8) 84_756 ?

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_3
_geom_angle_publ_flag
N1 Cu1 N1 91.8(4) 18_556 39_545 ?
N1 Cu1 N1 91.8(4) 18_556 . ?
N1 Cu1 N1 91.8(4) 39_545 . ?
N1 Cu1 O1 96.6(4) 18_556 18_556 ?
N1 Cu1 O1 170.0(5) 39_545 18_556 ?
N1 Cu1 O1 93.4(4) . 18_556 ?
N1 Cu1 O1 93.4(4) 18_556 39_545 ?
N1 Cu1 O1 96.6(4) 39_545 39_545 ?
N1 Cu1 O1 170.0(5) . 39_545 ?
O1 Cu1 O1 77.5(5) 18_556 39_545 ?
N1 Cu1 O1 170.0(5) 18_556 . ?
N1 Cu1 O1 93.4(4) 39_545 . ?
N1 Cu1 O1 96.5(4) . . ?
O1 Cu1 O1 77.5(5) 18_556 . ?
O1 Cu1 O1 77.5(5) 39_545 . ?
N2 Cu2 N2 91.0(3) . 66_764 ?
N2 Cu2 N2 89.0(3) . 18_556 ?
N2 Cu2 N2 180.0(5) 66_764 18_556 ?
N2 Cu2 N2 180.0(5) . 49_765 ?
N2 Cu2 N2 89.0(3) 66_764 49_765 ?
N2 Cu2 N2 91.0(3) 18_556 49_765 ?
N2 Cu2 N2 91.0(3) . 87_664 ?
N2 Cu2 N2 89.0(3) 66_764 87_664 ?
N2 Cu2 N2 91.0(3) 18_556 87_664 ?
N2 Cu2 N2 89.0(3) 49_765 87_664 ?
N2 Cu2 N2 89.0(3) . 39_545 ?
N2 Cu2 N2 91.0(3) 66_764 39_545 ?
N2 Cu2 N2 89.0(3) 18_556 39_545 ?
N2 Cu2 N2 91.0(3) 49_765 39_545 ?
N2 Cu2 N2 180.0(6) 87_664 39_545 ?
N4 C1 N3 110.2(10) . . ?
N4 C1 C2 122.4(10) . . ?
N3 C1 C2 127.4(10) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 119.5(7) . . ?
C7 C2 C1 120.5(7) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 Si1 118.9(5) . . ?
C6 C5 Si1 121.0(5) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
N2 N1 N4 106.9(9) . . ?
N2 N1 Cu1 127.9(8) . . ?
N4 N1 Cu1 125.2(8) . . ?
N3 N2 N1 109.9(9) . . ?
N3 N2 Cu2 127.9(7) . . ?
N1 N2 Cu2 122.0(7) . . ?
N2 N3 C1 106.6(9) . . ?
C1 N4 N1 106.4(9) . . ?
C5 Si1 C5 109.6(5) . 86_765 ?
C5 Si1 C5 109.2(7) . 5_565 ?
C5 Si1 C5 109.6(6) 86_765 5_565 ?
C5 Si1 C5 109.6(5) . 84_756 ?
C5 Si1 C5 109.2(10) 86_765 84_756 ?
C5 Si1 C5 109.6(6) 5_565 84_756 ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-4






_database_code_depnum_ccdc_archive 'CCDC 989925'
