# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
'Carles Miro Sabate'
'Erwann Jeanneau '
'Henri Delalu'
_publ_contact_author_name        'Carles Miro Sabate'
_publ_contact_author_email       carles_miro@hotmail.com

data_4
_database_code_depnum_ccdc_archive 'CCDC 852499'
#TrackingRef 'Compound 4.cif'

_exptl_special_details           
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.

Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details          
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.

# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape

# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace

# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "

# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html

# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a                   9.3890(10)
_cell_length_b                   10.6030(10)
_cell_length_c                   6.9241(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.750(10)
_cell_angle_gamma                90
_cell_volume                     672.31(13)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rb -0.9393 2.9676 17.1784 1.7888 9.6435 17.3151 5.1399 0.2748 1.5292 164.9340
3.4873 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            4

# Given Formula = C4 H4 N5 O2 Rb1
# Dc = 2.37 Fooo = 384.00 Mu = 73.25 M = 239.58
# Found Formula = C4 N5 Rb1
# Dc = 2.01 FOOO = 384.00 Mu = 72.85 M = 203.54

_chemical_formula_sum            'C4 N5 Rb1'
_chemical_formula_moiety         'C4 N5, Rb'
_chemical_compound_source        ?
_chemical_formula_weight         203.54

_cell_measurement_reflns_used    4423
_cell_measurement_theta_min      3.5696
_cell_measurement_theta_max      29.3636
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_min          0.172
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.363

_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             384
_exptl_absorpt_coefficient_mu    7.285

# Sheldrick geometric approximatio 0.23 0.29
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_T_max  0.165
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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)
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            9359
_reflns_number_total             1715
_diffrn_reflns_av_R_equivalents  0.051
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 1715
# Theoretical number of reflections is about 3722

_diffrn_reflns_theta_min         3.577
_diffrn_reflns_theta_max         29.426
_diffrn_measured_fraction_theta_max 0.922

_diffrn_reflns_theta_full        25.013
_diffrn_measured_fraction_theta_full 0.989

_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.61
_refine_diff_density_max         0.67

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         1715
_refine_ls_number_restraints     0
_refine_ls_number_parameters     92
_oxford_refine_ls_R_factor_ref   0.0344
_refine_ls_wR_factor_ref         0.0755
_refine_ls_goodness_of_fit_ref   0.9547
_refine_ls_shift/su_max          0.0005483
_refine_ls_shift/su_mean         0.0000292

# The values computed from all data
_oxford_reflns_number_all        1715
_refine_ls_R_factor_all          0.0344
_refine_ls_wR_factor_all         0.0755

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                1560
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_gt          0.0719

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.207E+04 0.334E+04 0.217E+04 981. 245.
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Oxford Diffraction, (2010). CrysAlisPro.

Oxford Diffraction, (2006). Gemini User Manual.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.

Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C.,
Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R.
(1999). J. App. Cryst. 32, 115-119.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R.,
Munksgaard, Copenhagen, 291-294.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Rb1 Rb 0.82194(3) 0.35368(2) 0.56256(4) 0.0127 1.0000 Uani . . . . . .
N2 N 0.7454(3) 0.6214(2) 0.4967(4) 0.0159 1.0000 Uani . . . . . .
N3 N 0.8847(3) 0.6340(2) 0.5909(4) 0.0163 1.0000 Uani . . . . . .
N4 N 0.9251(3) 0.7554(2) 0.6141(4) 0.0143 1.0000 Uani . . . . . .
C5 C 0.8061(3) 0.8240(3) 0.5302(4) 0.0141 1.0000 Uani . . . . . .
C6 C 0.6937(3) 0.7401(3) 0.4574(4) 0.0142 1.0000 Uani . . . . . .
C7 C 0.5460(3) 0.7633(3) 0.3552(4) 0.0168 1.0000 Uani . . . . . .
N8 N 0.4282(3) 0.7813(3) 0.2733(4) 0.0217 1.0000 Uani . . . . . .
C9 C 0.8079(3) 0.9581(3) 0.5233(4) 0.0159 1.0000 Uani . . . . . .
N10 N 0.8077(3) 1.0665(3) 0.5143(5) 0.0242 1.0000 Uani . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rb1 0.01105(16) 0.00986(15) 0.01644(16) -0.00004(8) 0.00114(10) 0.00008(8)
N2 0.0181(11) 0.0130(11) 0.0159(11) -0.0005(9) 0.0020(9) -0.0013(9)
N3 0.0160(12) 0.0142(11) 0.0186(12) -0.0002(9) 0.0034(9) 0.0007(9)
N4 0.0145(11) 0.0124(11) 0.0157(10) 0.0009(9) 0.0025(8) 0.0008(9)
C5 0.0170(12) 0.0112(12) 0.0145(11) -0.0003(10) 0.0042(10) -0.0002(10)
C6 0.0154(12) 0.0131(13) 0.0145(12) 0.0008(10) 0.0041(10) -0.0001(10)
C7 0.0172(13) 0.0183(13) 0.0156(12) -0.0003(10) 0.0052(10) 0.0003(11)
N8 0.0154(12) 0.0276(14) 0.0203(12) 0.0012(11) 0.0004(9) -0.0004(10)
C9 0.0156(12) 0.0133(13) 0.0186(12) 0.0011(11) 0.0034(10) -0.0007(10)
N10 0.0201(12) 0.0184(13) 0.0345(14) -0.0003(12) 0.0069(11) -0.0005(11)

_refine_ls_extinction_coef       23.1(13)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          4.65(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Rb1 . N2 . 2.938(3) yes
Rb1 . N3 . 3.028(3) yes
N2 . N3 . 1.333(4) yes
N2 . C6 . 1.355(4) yes
N3 . N4 . 1.341(3) yes
N4 . C5 . 1.352(4) yes
C5 . C6 . 1.387(4) yes
C5 . C9 . 1.423(4) yes
C6 . C7 . 1.432(4) yes
C7 . N8 . 1.143(4) yes
C9 . N10 . 1.151(4) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Rb1 . N3 . 25.76(7) yes
N3 . N2 . C6 . 105.9(2) yes
N3 . N2 . Rb1 . 80.89(15) yes
C6 . N2 . Rb1 . 173.2(2) yes
N2 . N3 . N4 . 112.1(2) yes
N2 . N3 . Rb1 . 73.36(14) yes
N4 . N3 . Rb1 . 174.51(19) yes
N3 . N4 . C5 . 106.2(2) yes
N4 . C5 . C6 . 107.5(3) yes
N4 . C5 . C9 . 122.5(3) yes
C6 . C5 . C9 . 130.0(3) yes
C5 . C6 . N2 . 108.2(3) yes
C5 . C6 . C7 . 130.2(3) yes
N2 . C6 . C7 . 121.6(3) yes
C6 . C7 . N8 . 179.6(3) yes
C5 . C9 . N10 . 178.7(3) yes

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 03/11/11 at 10:09:44
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
END
;

_iucr_refine_instruction_details_restraints 
;
#
# Punched on 03/11/11 at 10:09:44
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;

# Attachment 'Compound 6.cif'

data_6
_database_code_depnum_ccdc_archive 'CCDC 852500'
#TrackingRef 'Compound 6.cif'

_exptl_special_details           
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.

Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details          
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.

# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape

# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace

# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "

# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html

# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a                   9.2430(10)
_cell_length_b                   15.828(2)
_cell_length_c                   6.4632(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.230(10)
_cell_angle_gamma                90
_cell_volume                     945.5(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937
0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            2

# Given Formula = C8 Mg0.50 O0.50
# Dc = 1.24 Fooo = 420.00 Mu = 1.05 M = 176.30
# Found Formula = C4 H8 Mg0.50 N6 O10
# Dc = 1.42 FOOO = 420.00 Mu = 1.53 M = 202.29

_chemical_formula_sum            'C8 H16 Mg N10 O8'
_chemical_formula_moiety         'H12 Mg O6, 2(C4 N5), 2(H2 O)'
_chemical_compound_source        ?
_chemical_formula_weight         404.62

_cell_measurement_reflns_used    3338
_cell_measurement_theta_min      3.3980
_cell_measurement_theta_max      29.4289
_cell_measurement_temperature    100

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.123
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.655

_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.153

# Sheldrick geometric approximatio 0.97 0.98
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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)
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            9836
_reflns_number_total             2361
_diffrn_reflns_av_R_equivalents  0.080
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 2361
# Theoretical number of reflections is about 5266

_diffrn_reflns_theta_min         3.405
_diffrn_reflns_theta_max         29.492
_diffrn_measured_fraction_theta_max 0.899

_diffrn_reflns_theta_full        26.543
_diffrn_measured_fraction_theta_full 0.998

_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              8

_oxford_diffrn_Wilson_B_factor   2.24
_oxford_diffrn_Wilson_scale      0.04

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.77
_refine_diff_density_max         1.08

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     0
_refine_ls_number_parameters     125
_oxford_refine_ls_R_factor_ref   0.1062
_refine_ls_wR_factor_ref         0.1754
_refine_ls_goodness_of_fit_ref   1.0536
_refine_ls_shift/su_max          0.0001162
_refine_ls_shift/su_mean         0.0000136

# The values computed from all data
_oxford_reflns_number_all        2361
_refine_ls_R_factor_all          0.1062
_refine_ls_wR_factor_all         0.1754

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                2107
_refine_ls_R_factor_gt           0.0978
_refine_ls_wR_factor_gt          0.1733

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
805. 983. 534. 178.
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C.,
Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R.
(1999). J. App. Cryst. 32, 115-119.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Oxford Diffraction, (2002). CrysAlis RED.

Oxford Diffraction, (2006). Gemini User Manual.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mg1 Mg 1.0000 0.5000 1.0000 0.0166 1.0000 Uani S . . . . .
O11 O 0.8235(4) 0.5648(2) 1.1051(6) 0.0241 1.0000 Uani . . . . . .
H112 H 0.8002 0.6149 1.1047 0.0360 1.0000 Uiso R . . . . .
H111 H 0.7573 0.5378 1.1632 0.0358 1.0000 Uiso R . . . . .
O12 O 1.0968(4) 0.6130(2) 0.9210(5) 0.0208 1.0000 Uani . . . . . .
H122 H 1.1091 0.6252 0.8009 0.0314 1.0000 Uiso R . . . . .
H121 H 1.1829 0.6258 0.9364 0.0315 1.0000 Uiso R . . . . .
O10 O 0.9089(4) 0.4920(2) 0.7099(5) 0.0259 1.0000 Uani . . . . . .
H102 H 0.9140 0.4462 0.6481 0.0388 1.0000 Uiso R . . . . .
H101 H 0.8407 0.5249 0.6869 0.0392 1.0000 Uiso R . . . . .
O13 O 1.0911(4) 0.6620(2) 0.5109(6) 0.0276 1.0000 Uani . . . . . .
H132 H 1.1611 0.6931 0.4862 0.0411 1.0000 Uiso R . . . . .
H131 H 1.0067 0.6829 0.5135 0.0406 1.0000 Uiso R . . . . .
N1 N 0.3966(6) 0.5376(3) 0.7027(8) 0.0404 1.0000 Uani . . . . . .
C2 C 0.4863(6) 0.5855(3) 0.6700(8) 0.0246 1.0000 Uani . . . . . .
C3 C 0.5954(5) 0.6479(3) 0.6312(7) 0.0173 1.0000 Uani . . . . . .
N4 N 0.7341(4) 0.6299(3) 0.6052(6) 0.0187 1.0000 Uani . . . . . .
N5 N 0.8029(5) 0.7026(2) 0.5775(6) 0.0208 1.0000 Uani . . . . . .
N6 N 0.7117(4) 0.7671(3) 0.5870(6) 0.0187 1.0000 Uani . . . . . .
C7 C 0.5811(5) 0.7350(3) 0.6210(6) 0.0164 1.0000 Uani . . . . . .
C8 C 0.4523(5) 0.7836(3) 0.6370(7) 0.0209 1.0000 Uani . . . . . .
N9 N 0.3450(5) 0.8183(3) 0.6531(8) 0.0356 1.0000 Uani . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mg1 0.0177(10) 0.0171(10) 0.0152(10) -0.0015(9) -0.0022(9) 0.0003(9)
O11 0.0240(18) 0.0166(16) 0.032(2) 0.0044(15) 0.0066(15) 0.0028(14)
O12 0.0194(16) 0.0241(17) 0.0188(16) 0.0024(14) -0.0024(14) -0.0054(14)
O10 0.0349(19) 0.0249(19) 0.0178(16) -0.0036(14) -0.0099(15) 0.0061(17)
O13 0.0189(17) 0.039(2) 0.0248(18) 0.0055(16) 0.0017(15) -0.0003(16)
N1 0.048(3) 0.031(3) 0.043(3) -0.009(2) 0.015(3) -0.013(2)
C2 0.026(3) 0.026(3) 0.021(2) -0.005(2) 0.003(2) -0.002(2)
C3 0.018(2) 0.025(2) 0.0089(19) -0.0027(17) -0.0062(17) -0.004(2)
N4 0.0211(19) 0.025(2) 0.0096(17) -0.0011(15) -0.0048(15) -0.0021(17)
N5 0.031(2) 0.020(2) 0.0115(18) -0.0010(15) -0.0019(16) 0.0002(17)
N6 0.022(2) 0.024(2) 0.0107(18) -0.0006(15) -0.0048(15) -0.0010(16)
C7 0.012(2) 0.031(2) 0.0053(18) -0.0008(17) -0.0038(16) -0.0006(19)
C8 0.018(2) 0.033(3) 0.012(2) -0.0009(19) -0.0012(17) -0.001(2)
N9 0.032(3) 0.047(3) 0.028(2) -0.002(2) -0.006(2) 0.012(2)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.48(13)

loop_
_oxford_twin_element_scale_factors
0.829(2)
0.171(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mg1 . O11 2_767 2.046(3) yes
Mg1 . O10 2_767 2.056(3) yes
Mg1 . O12 2_767 2.065(3) yes
Mg1 . O11 . 2.046(3) yes
Mg1 . O12 . 2.065(3) yes
Mg1 . O10 . 2.056(3) yes
O11 . H112 . 0.822 no
O11 . H111 . 0.836 no
O12 . H122 . 0.808 no
O12 . H121 . 0.827 no
O10 . H102 . 0.829 no
O10 . H101 . 0.831 no
O13 . H132 . 0.829 no
O13 . H131 . 0.848 no
N1 . C2 . 1.144(7) yes
C2 . C3 . 1.434(7) yes
C3 . N4 . 1.325(6) yes
C3 . C7 . 1.386(7) yes
N4 . N5 . 1.328(5) yes
N5 . N6 . 1.325(5) yes
N6 . C7 . 1.329(6) yes
C7 . C8 . 1.421(6) yes
C8 . N9 . 1.139(6) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O11 2_767 Mg1 . O10 2_767 90.54(14) yes
O11 2_767 Mg1 . O12 2_767 89.72(13) yes
O10 2_767 Mg1 . O12 2_767 90.25(14) yes
O11 2_767 Mg1 . O11 . 179.994 yes
O10 2_767 Mg1 . O11 . 89.46(14) yes
O12 2_767 Mg1 . O11 . 90.28(13) yes
O11 2_767 Mg1 . O12 . 90.28(13) yes
O10 2_767 Mg1 . O12 . 89.75(14) yes
O12 2_767 Mg1 . O12 . 179.994 yes
O11 . Mg1 . O12 . 89.72(13) yes
O11 2_767 Mg1 . O10 . 89.46(14) yes
O10 2_767 Mg1 . O10 . 179.994 yes
O12 2_767 Mg1 . O10 . 89.75(13) yes
O11 . Mg1 . O10 . 90.54(14) yes
O12 . Mg1 . O10 . 90.25(13) yes
Mg1 . O11 . H112 . 133.8 no
Mg1 . O11 . H111 . 118.6 no
H112 . O11 . H111 . 107.6 no
Mg1 . O12 . H122 . 120.5 no
Mg1 . O12 . H121 . 126.9 no
H122 . O12 . H121 . 85.3 no
Mg1 . O10 . H102 . 118.0 no
Mg1 . O10 . H101 . 115.6 no
H102 . O10 . H101 . 120.5 no
H132 . O13 . H131 . 119.5 no
N1 . C2 . C3 . 178.0(6) yes
C2 . C3 . N4 . 123.7(4) yes
C2 . C3 . C7 . 128.7(4) yes
N4 . C3 . C7 . 107.5(4) yes
C3 . N4 . N5 . 107.1(4) yes
N4 . N5 . N6 . 110.9(4) yes
N5 . N6 . C7 . 107.0(4) yes
C3 . C7 . N6 . 107.5(4) yes
C3 . C7 . C8 . 128.0(4) yes
N6 . C7 . C8 . 124.5(4) yes
C7 . C8 . N9 . 175.9(6) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O11 . H112 . N6 3_565 171.02(15) 0.82 2.04 2.857(7) yes
O11 . H111 . N1 2_667 175.12(17) 0.84 2.05 2.886(7) yes
O12 . H122 . O13 . 167.00 0.81 1.97 2.762(7) yes
O12 . H121 . N9 3_665 144.79(16) 0.83 2.23 2.944(7) yes
O10 . H102 . O13 2_766 174.93(14) 0.83 2.00 2.824(7) yes
O10 . H101 . N4 . 160.00 0.83 2.00 2.796(7) yes
O13 . H131 . N5 . 163.00 0.85 1.95 2.775(7) yes

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 24/06/11 at 11:04:12
#
#LIST 12
BLOCK SCALE X'S, U'S
SUMFIX ELEMENT SCALES
RIDE O ( 2,X'S) H ( 22,X'S) H ( 21,X'S)
RIDE O ( 3,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE O ( 4,X'S) H ( 42,X'S) H ( 41,X'S)
RIDE O ( 5,X'S) H ( 52,X'S) H ( 51,X'S)
END
;

_iucr_refine_instruction_details_restraints 
;
#
# Punched on 24/06/11 at 11:04:12
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;

# Attachment 'Compound 8b.cif'

data_8b
_database_code_depnum_ccdc_archive 'CCDC 852501'
#TrackingRef 'Compound 8b.cif'

_exptl_special_details           
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.

Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details          
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.

# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape

# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace

# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "

# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html

# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a                   6.9498(5)
_cell_length_b                   17.7690(10)
_cell_length_c                   13.8575(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.982(6)
_cell_angle_gamma                90
_cell_volume                     1708.96(19)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cs -0.3680 2.1192 20.3892 3.5690 19.1062 0.3107 10.6620 24.3879 1.4953 213.9040
3.3352 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sr -1.5307 3.2498 17.5663 1.5564 9.8184 14.0988 5.4220 0.1664 2.6694 132.3760
2.5064 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_formula_units_Z            2

# Given Formula = C7 H10.50 Cs1.75 N10.50 O7 Sr1.50
# Dc = 2.79 Fooo = 864.00 Mu = 84.34 M = 717.74
# Found Formula = C8 H10 N8 O8 Sr1
# Dc = 1.69 FOOO = 864.00 Mu = 32.10 M = 433.84

_chemical_formula_sum            'C16 H20 N16 O16 Sr2'
_chemical_formula_moiety         'C16 H20 N16 O16 Sr2'
_chemical_compound_source        ?
_chemical_formula_weight         867.72

_cell_measurement_reflns_used    12970
_cell_measurement_theta_min      3.4062
_cell_measurement_theta_max      29.4767
_cell_measurement_temperature    100

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.123
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_max          0.458

_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    3.210

# Sheldrick geometric approximatio 0.56 0.67
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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)
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measurement_method       \w

# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            39094
_reflns_number_total             4505
_diffrn_reflns_av_R_equivalents  0.000
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 4505
# Theoretical number of reflections is about 9560

_diffrn_reflns_theta_min         3.413
_diffrn_reflns_theta_max         29.540
_diffrn_measured_fraction_theta_max 0.943

_diffrn_reflns_theta_full        25.109
_diffrn_measured_fraction_theta_full 0.995

_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -9
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.48
_refine_diff_density_max         1.19

# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold

# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     0
_refine_ls_number_parameters     226
_oxford_refine_ls_R_factor_ref   0.0707
_refine_ls_wR_factor_ref         0.1362
_refine_ls_goodness_of_fit_ref   0.9544
_refine_ls_shift/su_max          0.0008989
_refine_ls_shift/su_mean         0.0000332

# The values computed from all data
_oxford_reflns_number_all        4505
_refine_ls_R_factor_all          0.0707
_refine_ls_wR_factor_all         0.1362

# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression     I>2.0\s(I)
_reflns_number_gt                3838
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_gt          0.1212

# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.219E+05 0.363E+05 0.225E+05 0.999E+04 0.251E+04
;
# Insert your own references if required - in alphabetical order
_publ_section_references         
;
Oxford Diffraction, (2010). CrysAlisPro.

Oxford Diffraction, (2006). Gemini User Manual.

Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.

Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C.,
Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R.
(1999). J. App. Cryst. 32, 115-119.

Watkin D.J. (1994).
Acta Cryst, A50, 411-437.

Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
N1 N 0.4789(6) 0.5896(2) 0.3393(3) 0.0264 1.0000 Uani . . . . . .
C2 C 0.4995(6) 0.6531(3) 0.3502(3) 0.0217 1.0000 Uani . . . . . .
C3 C 0.5311(6) 0.7314(2) 0.3659(3) 0.0184 1.0000 Uani . . . . . .
N4 N 0.4904(5) 0.7832(2) 0.2965(3) 0.0208 1.0000 Uani . . . . . .
N5 N 0.5376(5) 0.8496(2) 0.3363(3) 0.0219 1.0000 Uani . . . . . .
N6 N 0.6091(5) 0.8416(2) 0.4278(3) 0.0212 1.0000 Uani . . . . . .
C7 C 0.6079(6) 0.7678(3) 0.4477(3) 0.0189 1.0000 Uani . . . . . .
C8 C 0.6830(6) 0.7323(3) 0.5384(3) 0.0217 1.0000 Uani . . . . . .
O9 O 0.7848(6) 0.7754(3) 0.6014(3) 0.0405 1.0000 Uani . . . . . .
O10 O 0.6521(5) 0.6646(2) 0.5509(2) 0.0256 1.0000 Uani . . . . . .
N11 N 0.2782(6) 0.8095(2) 0.6065(3) 0.0277 1.0000 Uani . . . . . .
C12 C 0.3573(6) 0.8200(3) 0.6802(3) 0.0216 1.0000 Uani . . . . . .
C13 C 0.4458(6) 0.8339(2) 0.7735(3) 0.0188 1.0000 Uani . . . . . .
N14 N 0.4554(5) 0.9033(2) 0.8106(3) 0.0206 1.0000 Uani . . . . . .
N15 N 0.5288(6) 0.8965(2) 0.9013(3) 0.0210 1.0000 Uani . . . . . .
N16 N 0.5687(5) 0.8244(2) 0.9221(2) 0.0177 1.0000 Uani . . . . . .
C17 C 0.5183(5) 0.7840(2) 0.8429(3) 0.0160 1.0000 Uani . . . . . .
C18 C 0.5328(6) 0.7010(2) 0.8354(3) 0.0172 1.0000 Uani . . . . . .
O19 O 0.5990(5) 0.6642(2) 0.9135(3) 0.0327 1.0000 Uani . . . . . .
O20 O 0.4823(5) 0.67078(18) 0.7576(2) 0.0227 1.0000 Uani . . . . . .
O21 O 0.1797(5) 0.63608(19) 0.6122(2) 0.0253 1.0000 Uani . . . . . .
O22 O 0.7244(4) 0.50496(17) 0.5056(2) 0.0196 1.0000 Uani . . . . . .
O23 O 0.2752(5) 0.51884(19) 0.7727(3) 0.0283 1.0000 Uani . . . . . .
O24 O 0.7822(5) 0.5379(2) 0.7541(3) 0.0336 1.0000 Uani . . . . . .
Sr1 Sr 0.49386(6) 0.56258(2) 0.63873(3) 0.0179 1.0000 Uani . . . . . .
H232 H 0.3283 0.5284 0.8247 0.0428 1.0000 Uiso R . . . . .
H231 H 0.1978 0.4873 0.7496 0.0430 1.0000 Uiso R . . . . .
H212 H 0.1453 0.6591 0.5618 0.0390 1.0000 Uiso R . . . . .
H211 H 0.1674 0.6644 0.6593 0.0393 1.0000 Uiso R . . . . .
H222 H 0.7959 0.4748 0.5348 0.0291 1.0000 Uiso R . . . . .
H91 H 0.8356 0.7567 0.6534 0.0599 1.0000 Uiso R . . . . .
H221 H 0.7822 0.5430 0.4915 0.0293 1.0000 Uiso R . . . . .
H242 H 0.8534 0.5731 0.7707 0.0512 1.0000 Uiso R . . . . .
H241 H 0.7808 0.5001 0.7878 0.0514 1.0000 Uiso R . . . . .
H191 H 0.6074 0.6163 0.9112 0.0481 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0229(18) 0.027(2) 0.029(2) -0.0032(16) 0.0024(15) 0.0009(15)
C2 0.0135(17) 0.031(2) 0.021(2) 0.0001(17) 0.0007(15) 0.0033(16)
C3 0.0126(17) 0.024(2) 0.0185(19) 0.0015(16) 0.0014(14) 0.0025(15)
N4 0.0183(16) 0.0265(19) 0.0174(17) 0.0004(14) 0.0000(13) 0.0005(14)
N5 0.0198(17) 0.0251(18) 0.0208(18) 0.0012(14) 0.0004(14) -0.0033(14)
N6 0.0165(16) 0.0290(19) 0.0178(17) 0.0035(14) -0.0009(13) -0.0050(14)
C7 0.0129(17) 0.025(2) 0.0184(19) 0.0018(16) 0.0008(14) -0.0034(15)
C8 0.0144(18) 0.032(2) 0.0190(19) 0.0026(17) 0.0025(15) 0.0009(16)
O9 0.033(2) 0.054(3) 0.034(2) 0.0010(18) -0.0049(16) 0.0013(18)
O10 0.0233(15) 0.0314(17) 0.0221(15) 0.0022(13) 0.0009(12) 0.0038(13)
N11 0.0259(19) 0.033(2) 0.024(2) 0.0008(16) -0.0067(15) 0.0009(17)
C12 0.0174(18) 0.027(2) 0.020(2) 0.0003(17) 0.0001(15) 0.0018(16)
C13 0.0140(17) 0.023(2) 0.0193(19) 0.0007(16) -0.0023(14) -0.0007(15)
N14 0.0211(17) 0.0236(18) 0.0170(17) -0.0004(14) -0.0008(13) 0.0037(14)
N15 0.0252(18) 0.0197(17) 0.0179(17) -0.0023(14) 0.0005(14) -0.0020(14)
N16 0.0165(15) 0.0216(17) 0.0147(16) -0.0018(13) -0.0007(12) -0.0004(13)
C17 0.0125(16) 0.0225(19) 0.0130(17) 0.0012(15) 0.0007(13) -0.0011(14)
C18 0.0138(17) 0.0207(19) 0.0170(18) -0.0017(15) -0.0005(14) -0.0009(14)
O19 0.0344(19) 0.0323(19) 0.0309(19) 0.0023(15) -0.0023(15) 0.0028(16)
O20 0.0270(16) 0.0213(15) 0.0193(15) -0.0022(12) -0.0038(12) -0.0014(12)
O21 0.0278(16) 0.0286(17) 0.0186(15) -0.0035(13) -0.0065(12) 0.0080(13)
O22 0.0202(14) 0.0175(14) 0.0210(14) -0.0015(11) 0.0001(11) 0.0011(11)
O23 0.0263(16) 0.0253(17) 0.0335(19) -0.0040(14) 0.0041(14) -0.0050(13)
O24 0.0272(18) 0.0252(17) 0.047(2) -0.0016(16) -0.0141(16) -0.0007(14)
Sr1 0.01636(19) 0.0194(2) 0.0176(2) -0.00377(14) -0.00095(14) 0.00080(14)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          12.2(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
N1 . C2 . 1.148(6) yes
C2 . C3 . 1.422(6) yes
C3 . N4 . 1.350(5) yes
C3 . C7 . 1.388(6) yes
N4 . N5 . 1.336(5) yes
N5 . N6 . 1.346(5) yes
N6 . C7 . 1.341(6) yes
C7 . C8 . 1.477(6) yes
C8 . O9 . 1.336(6) yes
C8 . O10 . 1.235(6) yes
O9 . H91 . 0.854 no
O10 . Sr1 . 2.473(3) yes
N11 . C12 . 1.150(6) yes
C12 . C13 . 1.424(6) yes
C13 . N14 . 1.337(6) yes
C13 . C17 . 1.383(6) yes
N14 . N15 . 1.338(5) yes
N15 . N16 . 1.338(5) yes
N16 . C17 . 1.343(5) yes
C17 . C18 . 1.482(6) yes
C18 . O19 . 1.326(5) yes
C18 . O20 . 1.239(5) yes
O19 . H191 . 0.854 no
O20 . Sr1 . 2.536(3) yes
O21 . H212 . 0.833 no
O21 . H211 . 0.831 no
O21 . Sr1 . 2.554(3) yes
O22 . H222 . 0.822 no
O22 . H221 . 0.816 no
O22 . Sr1 . 2.706(3) yes
O23 . H232 . 0.810 no
O23 . H231 . 0.829 no
O23 . Sr1 . 2.579(3) yes
O24 . H242 . 0.823 no
O24 . H241 . 0.818 no
O24 . Sr1 . 2.536(3) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . C2 . C3 . 177.9(5) yes
C2 . C3 . N4 . 122.2(4) yes
C2 . C3 . C7 . 129.0(4) yes
N4 . C3 . C7 . 108.8(4) yes
C3 . N4 . N5 . 105.7(3) yes
N4 . N5 . N6 . 111.5(4) yes
N5 . N6 . C7 . 106.9(4) yes
C3 . C7 . N6 . 107.1(4) yes
C3 . C7 . C8 . 126.9(4) yes
N6 . C7 . C8 . 126.0(4) yes
C7 . C8 . O9 . 117.6(4) yes
C7 . C8 . O10 . 118.6(4) yes
O9 . C8 . O10 . 123.8(4) yes
C8 . O9 . H91 . 120.8 no
C8 . O10 . Sr1 . 150.2(3) yes
N11 . C12 . C13 . 177.0(5) yes
C12 . C13 . N14 . 121.3(4) yes
C12 . C13 . C17 . 130.1(4) yes
N14 . C13 . C17 . 108.4(4) yes
C13 . N14 . N15 . 106.6(4) yes
N14 . N15 . N16 . 110.7(3) yes
N15 . N16 . C17 . 107.0(3) yes
C13 . C17 . N16 . 107.2(4) yes
C13 . C17 . C18 . 127.8(4) yes
N16 . C17 . C18 . 124.9(4) yes
C17 . C18 . O19 . 117.2(4) yes
C17 . C18 . O20 . 118.4(4) yes
O19 . C18 . O20 . 124.5(4) yes
C18 . O19 . H191 . 119.0 no
C18 . O20 . Sr1 . 151.3(3) yes
H212 . O21 . H211 . 108.9 no
H212 . O21 . Sr1 . 125.3 no
H211 . O21 . Sr1 . 108.5 no
H222 . O22 . H221 . 111.4 no
H222 . O22 . Sr1 . 106.0 no
H221 . O22 . Sr1 . 99.6 no
H232 . O23 . H231 . 137.8 no
H232 . O23 . Sr1 . 108.6 no
H231 . O23 . Sr1 . 108.7 no
H242 . O24 . H241 . 119.3 no
H242 . O24 . Sr1 . 119.2 no
H241 . O24 . Sr1 . 118.0 no
O24 . Sr1 . O21 . 145.15(11) yes
O24 . Sr1 . O23 . 88.27(12) yes
O21 . Sr1 . O23 . 74.12(11) yes
O24 . Sr1 . O20 . 76.85(11) yes
O21 . Sr1 . O20 . 69.52(10) yes
O23 . Sr1 . O20 . 73.80(11) yes
O24 . Sr1 . O10 . 94.61(12) yes
O21 . Sr1 . O10 . 87.31(11) yes
O23 . Sr1 . O10 . 150.32(11) yes
O20 . Sr1 . O10 . 78.12(11) yes
O24 . Sr1 . O22 . 83.56(11) yes
O21 . Sr1 . O22 . 128.85(10) yes
O23 . Sr1 . O22 . 140.20(10) yes
O20 . Sr1 . O22 . 140.31(10) yes
O10 . Sr1 . O22 . 69.37(10) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O23 . H231 . N14 3_546 171.90(15) 0.829 1.991 2.814(6) yes
O21 . H212 . N15 4_464 127.61(11) 0.833 2.528 3.107(6) yes
O21 . H212 . N16 4_464 158.75(14) 0.833 2.002 2.796(6) yes
O21 . H211 . N4 4_465 153.81(12) 0.831 2.498 3.265(6) yes
O22 . H222 . N15 3_646 176.19(14) 0.822 2.024 2.845(6) yes
O9 . H91 . N4 4_565 174.46(14) 0.854 2.317 3.168(6) yes
O22 . H221 . N15 4_564 149.54(11) 0.816 2.424 3.154(6) yes
O24 . H242 . N5 4_565 169.21(15) 0.823 2.058 2.870(6) yes

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 27/10/11 at 15:38:35
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE O ( 9,X'S) H ( 91,X'S)
RIDE O ( 19,X'S) H ( 191,X'S)
RIDE O ( 21,X'S) H ( 212,X'S) H ( 211,X'S)
RIDE O ( 22,X'S) H ( 222,X'S) H ( 221,X'S)
RIDE O ( 23,X'S) H ( 232,X'S) H ( 231,X'S)
RIDE O ( 24,X'S) H ( 242,X'S) H ( 241,X'S)
END
;

_iucr_refine_instruction_details_restraints 
;
#
# Punched on 27/10/11 at 15:38:35
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;

# 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 -0.015 0.500 0.000 97 23 ' '
2 0.066 0.000 0.500 97 23 ' '
_platon_squeeze_details          
;
;