# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_150K
_database_code_depnum_ccdc_archive 'CCDC 1420162'
_audit_update_record             
;
2015-08-21 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_150K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The  chemistry/geometry is well understood and the hydrogen atoms were refined  with restraints (prior to inclusion in the final refinement using a riding  model) and are within expected parameters.
;

# Added during the CSD deposition process: Friday 21st of August 2015 07:23:07 PM
# end Validation Reply Form

#==============================================================================
_audit_creation_date             12-11-19
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 040iec11
_chemical_name_systematic        'guanidinium cadmium formate'
_chemical_melting_point          'not measured'

_cell_length_a                   9.2335(6)
_cell_length_b                   9.2335(6)
_cell_length_c                   19.2916(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1424.38(15)

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3 c '
_symmetry_space_group_name_Hall  '-R 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x+y,y,z+1/2
x-y,-y,-z+1/2
-x+y+1/3,y+2/3,z+7/6
x-y+1/3,-y+2/3,-z+7/6
-x+y+2/3,y+1/3,z+5/6
x-y+2/3,-y+1/3,-z+5/6
x,x-y,z+1/2
-x,-x+y,-z+1/2
x+1/3,x-y+2/3,z+7/6
-x+1/3,-x+y+2/3,-z+7/6
x+2/3,x-y+1/3,z+5/6
-x+2/3,-x+y+1/3,-z+5/6
-y,-x,z+1/2
y,x,-z+1/2
-y+1/3,-x+2/3,z+7/6
y+1/3,x+2/3,-z+7/6
-y+2/3,-x+1/3,z+5/6
y+2/3,x+1/3,-z+5/6

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'
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'
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'
Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825
5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.15 Fooo =    900.00 Mu =     23.11 M =     51.26
# Found Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.15 FOOO =    900.00 Mu =     23.11 M =     51.26

_chemical_formula_sum            'C4 H9 Cd1 N3 O6'
_chemical_formula_moiety         'C3 H3 Cd O6, C H6 N3 '
_chemical_compound_source        'not measured'
_chemical_formula_weight         307.53


_cell_measurement_reflns_used    701
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    2.151
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    2.311

# Sheldrick geometric approximatio 0.63 0.63 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_T_max  0.63
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_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      150
_diffrn_reflns_number            3262
_reflns_number_total             360
_diffrn_reflns_av_R_equivalents  0.036
# Number of reflections without Friedels Law is 1129 
# Number of reflections with Friedels Law is 360 
# Theoretical number of reflections is about 360


_diffrn_reflns_theta_min         5.437
_diffrn_reflns_theta_max         27.408
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.408
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -10
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   1.62
_oxford_diffrn_Wilson_scale      120.05

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

_refine_diff_density_min         -0.92
_refine_diff_density_max         0.54


# 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>-3.0\s(I)
_refine_ls_number_reflns         360
_refine_ls_number_restraints     0
_refine_ls_number_parameters     24
_oxford_refine_ls_R_factor_ref   0.0375
_refine_ls_wR_factor_ref         0.0836
_refine_ls_goodness_of_fit_ref   0.8987
_refine_ls_shift/su_max          0.0001202
_refine_ls_shift/su_mean         0.0000135


# The values computed from all data 
_oxford_reflns_number_all        360
_refine_ls_R_factor_all          0.0375
_refine_ls_wR_factor_all         0.0836

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                295
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_gt          0.0726

# 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    noref # 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/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 7.43 11.4 5.89 1.61 
;

# 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
Cd1 Cd 0.6667 0.3333 0.3333 0.0173 1.0000 Uani S T . . . .
O2 O 0.8851(3) 0.5381(3) 0.39440(12) 0.0259 1.0000 Uani . . . . . .
C4 C 0.8866(5) 0.6667 0.4167 0.0269 1.0000 Uani S T . . . .
C3 C 0.6667 0.3333 0.0833 0.0243 1.0000 Uani S T . . . .
N5 N 0.8100(4) 0.3333 0.0833 0.0298 1.0000 Uani S T . . . .
H42 H 0.7818 0.6667 0.4167 0.0380 1.0000 Uiso . . . . . .
H52 H 0.8095 0.2404 0.0803 0.0479 1.0000 Uiso . . . . . .
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
Cd1 0.0152(3) 0.0152(3) 0.0216(4) 0.0000 0.0000 0.00758(15)
O2 0.0226(11) 0.0217(11) 0.0343(11) -0.0086(10) -0.0056(9) 0.0117(9)
C4 0.0211(16) 0.027(2) 0.034(2) -0.005(2) -0.0027(10) 0.0136(12)
C3 0.023(3) 0.023(3) 0.027(5) 0.0000 0.0000 0.0115(15)
N5 0.0216(14) 0.019(2) 0.048(2) -0.0022(17) -0.0011(9) 0.0096(10)

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.09014(8)
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
Cd1 . O2 16_545 2.284(2) yes
Cd1 . O2 13_665 2.284(2) yes
Cd1 . O2 7_655 2.284(2) yes
Cd1 . O2 10_555 2.284(2) yes
Cd1 . O2 4_655 2.284(2) yes
Cd1 . O2 . 2.284(2) yes
O2 . C4 . 1.255(3) yes
C4 . H42 . 0.968 no
C3 . N5 34_544 1.324(4) yes
C3 . N5 28_654 1.324(4) yes
C3 . N5 . 1.324(4) yes
N5 . H52 22_554 0.858 no
N5 . H52 . 0.858 no
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
O2 16_545 Cd1 . O2 13_665 179.995 yes
O2 16_545 Cd1 . O2 7_655 84.21(8) yes
O2 13_665 Cd1 . O2 7_655 95.79(8) yes
O2 16_545 Cd1 . O2 10_555 95.79(8) yes
O2 13_665 Cd1 . O2 10_555 84.21(8) yes
O2 7_655 Cd1 . O2 10_555 179.995 yes
O2 16_545 Cd1 . O2 4_655 95.79(8) yes
O2 13_665 Cd1 . O2 4_655 84.21(8) yes
O2 7_655 Cd1 . O2 4_655 84.21(8) yes
O2 10_555 Cd1 . O2 4_655 95.79(8) yes
O2 16_545 Cd1 . O2 . 84.21(8) yes
O2 13_665 Cd1 . O2 . 95.79(8) yes
O2 7_655 Cd1 . O2 . 95.79(8) yes
O2 10_555 Cd1 . O2 . 84.21(8) yes
O2 4_655 Cd1 . O2 . 179.995 yes
Cd1 . O2 . C4 . 123.2(2) yes
O2 . C4 . O2 24_565 125.1(5) yes
O2 . C4 . H42 . 117.5 no
O2 24_565 C4 . H42 . 117.5 no
N5 34_544 C3 . N5 28_654 120.000(3) yes
N5 34_544 C3 . N5 . 120.000(3) yes
N5 28_654 C3 . N5 . 120.000(6) yes
C3 . N5 . H52 22_554 119.7 no
C3 . N5 . H52 . 119.7 no
H52 22_554 N5 . H52 . 120.7 no
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
N5 . H52 . O2 9_644 172.84 0.858 2.065 2.9182(12) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/11/12 at 18:39:33
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/11/12 at 18:39:33
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_250K
_database_code_depnum_ccdc_archive 'CCDC 1420163'
_audit_update_record             
;
2015-08-21 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_250K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The  chemistry/geometry is well understood and the hydrogen atoms were refined  with restraints (prior to inclusion in the final refinement using a riding  model) and are within expected parameters.
;

# Added during the CSD deposition process: Friday 21st of August 2015 07:23:07 PM
# end Validation Reply Form

#==============================================================================
_audit_creation_date             12-11-19
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 041iec11
_chemical_name_systematic        'guanidinium cadmium formate'
_chemical_melting_point          'not measured'

_cell_length_a                   9.2172(4)
_cell_length_b                   9.2172(4)
_cell_length_c                   19.4982(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1434.56(11)

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3 c '
_symmetry_space_group_name_Hall  '-R 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x+y,y,z+1/2
x-y,-y,-z+1/2
-x+y+1/3,y+2/3,z+7/6
x-y+1/3,-y+2/3,-z+7/6
-x+y+2/3,y+1/3,z+5/6
x-y+2/3,-y+1/3,-z+5/6
x,x-y,z+1/2
-x,-x+y,-z+1/2
x+1/3,x-y+2/3,z+7/6
-x+1/3,-x+y+2/3,-z+7/6
x+2/3,x-y+1/3,z+5/6
-x+2/3,-x+y+1/3,-z+5/6
-y,-x,z+1/2
y,x,-z+1/2
-y+1/3,-x+2/3,z+7/6
y+1/3,x+2/3,-z+7/6
-y+2/3,-x+1/3,z+5/6
y+2/3,x+1/3,-z+5/6

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'
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'
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'
Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825
5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.14 Fooo =    900.00 Mu =     22.94 M =     51.26
# Found Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.14 FOOO =    900.00 Mu =     22.94 M =     51.26

_chemical_formula_sum            'C4 H9 Cd1 N3 O6'
_chemical_formula_moiety         'C3 H3 Cd O6, C H6 N3 '
_chemical_compound_source        'not measured'
_chemical_formula_weight         307.53


_cell_measurement_reflns_used    706
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    250

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    2.294

# Sheldrick geometric approximatio 0.63 0.63 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.63
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Refinement of 150 K structure'
_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      250
_diffrn_reflns_number            3280
_reflns_number_total             365
_diffrn_reflns_av_R_equivalents  0.024
# Number of reflections without Friedels Law is 1129  
# Number of reflections with Friedels Law is 365 
# Theoretical number of reflections is about 365 


_diffrn_reflns_theta_min         5.424
_diffrn_reflns_theta_max         27.465
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.465
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -10
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   1.42
_oxford_diffrn_Wilson_scale      64.67

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

_refine_diff_density_min         -0.79
_refine_diff_density_max         0.49


# 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>-3.0\s(I)
_refine_ls_number_reflns         365
_refine_ls_number_restraints     0
_refine_ls_number_parameters     25
_oxford_refine_ls_R_factor_ref   0.0242
_refine_ls_wR_factor_ref         0.0458
_refine_ls_goodness_of_fit_ref   1.0118
_refine_ls_shift/su_max          0.0001730
_refine_ls_shift/su_mean         0.0000200


# The values computed from all data 
_oxford_reflns_number_all        365
_refine_ls_R_factor_all          0.0242
_refine_ls_wR_factor_all         0.0458

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                307
_refine_ls_R_factor_gt           0.0191
_refine_ls_wR_factor_gt          0.0415

# 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    noref # 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/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.17 5.26 1.59 
;

# 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
Cd1 Cd 0.6667 0.3333 0.3333 0.0166 1.0000 Uani S T . . . .
O2 O 0.8845(3) 0.5392(2) 0.39437(10) 0.0293 1.0000 Uani . . . . . .
C4 C 0.8871(4) 0.6667 0.4167 0.0298 1.0000 Uani S T . . . .
C3 C 0.6667 0.3333 0.0833 0.0241 1.0000 Uani S T . . . .
N5 N 0.8098(4) 0.3333 0.0833 0.0359 1.0000 Uani S T . . . .
H42 H 0.7818 0.6667 0.4167 0.0380 1.0000 Uiso . . . . . .
H52 H 0.8095 0.2404 0.0803 0.0479 1.0000 Uiso . . . . . .
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
Cd1 0.0139(3) 0.0139(3) 0.0218(3) 0.0000 0.0000 0.00697(13)
O2 0.0249(10) 0.0239(11) 0.0403(11) -0.0123(9) -0.0092(9) 0.0132(9)
C4 0.0207(14) 0.032(2) 0.041(2) -0.0127(19) -0.0063(9) 0.0160(11)
C3 0.020(2) 0.020(2) 0.031(4) 0.0000 0.0000 0.0102(10)
N5 0.0201(13) 0.0243(19) 0.065(3) -0.0070(18) -0.0035(9) 0.0122(9)

_refine_ls_extinction_coef       97(6)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.13092(18)
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
Cd1 . O2 16_545 2.2890(19) yes
Cd1 . O2 4_655 2.2890(19) yes
Cd1 . O2 10_555 2.2890(19) yes
Cd1 . O2 13_665 2.2890(19) yes
Cd1 . O2 7_655 2.2890(19) yes
Cd1 . O2 . 2.2890(19) yes
O2 . C4 . 1.242(3) yes
C4 . H42 . 0.970 no
C3 . N5 7_655 1.320(4) yes
C3 . N5 13_665 1.320(4) yes
C3 . N5 . 1.320(4) yes
N5 . H52 22_554 0.857 no
N5 . H52 . 0.857 no
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
O2 16_545 Cd1 . O2 4_655 95.42(7) yes
O2 16_545 Cd1 . O2 10_555 95.42(7) yes
O2 4_655 Cd1 . O2 10_555 95.42(7) yes
O2 16_545 Cd1 . O2 13_665 179.995 yes
O2 4_655 Cd1 . O2 13_665 84.58(7) yes
O2 10_555 Cd1 . O2 13_665 84.58(7) yes
O2 16_545 Cd1 . O2 7_655 84.58(7) yes
O2 4_655 Cd1 . O2 7_655 84.58(7) yes
O2 10_555 Cd1 . O2 7_655 179.995 yes
O2 13_665 Cd1 . O2 7_655 95.42(7) yes
O2 16_545 Cd1 . O2 . 84.58(7) yes
O2 4_655 Cd1 . O2 . 179.995 yes
O2 10_555 Cd1 . O2 . 84.58(7) yes
O2 13_665 Cd1 . O2 . 95.42(7) yes
O2 7_655 Cd1 . O2 . 95.42(7) yes
Cd1 . O2 . C4 . 124.1(2) yes
O2 . C4 . O2 24_565 126.0(4) yes
O2 . C4 . H42 . 117.0 no
O2 24_565 C4 . H42 . 117.0 no
N5 7_655 C3 . N5 13_665 120.000 yes
N5 7_655 C3 . N5 . 120.000 yes
N5 13_665 C3 . N5 . 120.000(4) yes
C3 . N5 . H52 22_554 119.8 no
C3 . N5 . H52 . 119.8 no
H52 22_554 N5 . H52 . 120.5 no
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
N5 . H52 . O2 9_644 172.67 0.857 2.072 2.9247(10) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/11/12 at 18:35:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/11/12 at 18:35:57
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_300K
_database_code_depnum_ccdc_archive 'CCDC 1420164'
_audit_update_record             
;
2015-08-21 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_300K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The  chemistry/geometry is well understood and the hydrogen atoms were refined  with restraints (prior to inclusion in the final refinement using a riding  model) and are within expected parameters.
;

# Added during the CSD deposition process: Friday 21st of August 2015 07:23:07 PM
# end Validation Reply Form

#==============================================================================
_audit_creation_date             12-11-19
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 050iec11
_chemical_name_systematic        'guanidinium cadmium formate'
_chemical_melting_point          'not measured'

_cell_length_a                   9.2146(3)
_cell_length_b                   9.2146(3)
_cell_length_c                   19.6072(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1441.77(13)

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 c '
_symmetry_space_group_name_Hall  '-R 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
x-y,-y,-z+1/2
-x+y,y,z+1/2
x-y+1/3,-y+2/3,-z+7/6
-x+y+1/3,y+2/3,z+7/6
x-y+2/3,-y+1/3,-z+5/6
-x+y+2/3,y+1/3,z+5/6
y,x,-z+1/2
-y,-x,z+1/2
y+1/3,x+2/3,-z+7/6
-y+1/3,-x+2/3,z+7/6
y+2/3,x+1/3,-z+5/6
-y+2/3,-x+1/3,z+5/6
y,-x+y,-z
-y,x-y,z
y+1/3,-x+y+2/3,-z+2/3
-y+1/3,x-y+2/3,z+2/3
y+2/3,-x+y+1/3,-z+1/3
-y+2/3,x-y+1/3,z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x,-x+y,-z+1/2
x,x-y,z+1/2
-x+1/3,-x+y+2/3,-z+7/6
x+1/3,x-y+2/3,z+7/6
-x+2/3,-x+y+1/3,-z+5/6
x+2/3,x-y+1/3,z+5/6

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'
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'
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'
Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825
5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.13 Fooo =    900.00 Mu =     22.83 M =     51.26
# Found Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.13 FOOO =    900.00 Mu =     22.83 M =     51.26

_chemical_formula_sum            'C4 H9 Cd1 N3 O6'
_chemical_formula_moiety         'C3 H3 Cd O6, C H6 N3 '
_chemical_compound_source        'not measured'
_chemical_formula_weight         307.53


_cell_measurement_reflns_used    5098
_cell_measurement_theta_min      3
_cell_measurement_theta_max      31
_cell_measurement_temperature    300

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    2.283

# Sheldrick geometric approximatio 0.71 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.93
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Refinement of 150 K structure'
_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      300
_diffrn_reflns_number            11511
_reflns_number_total             485
_diffrn_reflns_av_R_equivalents  0.049
# Number of reflections with Friedels Law is 485 
# Theoretical number of reflections is about 988 


_diffrn_reflns_theta_min         3.292
_diffrn_reflns_theta_max         30.626
_diffrn_measured_fraction_theta_max 0.976

_diffrn_reflns_theta_full        29.094
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -11
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   1.27
_oxford_diffrn_Wilson_scale      0.14

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

_refine_diff_density_min         -0.83
_refine_diff_density_max         0.80


# 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         485
_refine_ls_number_restraints     0
_refine_ls_number_parameters     25
_oxford_refine_ls_R_factor_ref   0.0302
_refine_ls_wR_factor_ref         0.0480
_refine_ls_goodness_of_fit_ref   0.8076
_refine_ls_shift/su_max          0.0000993
_refine_ls_shift/su_mean         0.0000127


# The values computed from all data 
_oxford_reflns_number_all        485
_refine_ls_R_factor_all          0.0302
_refine_ls_wR_factor_all         0.0480

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                389
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_gt          0.0397

# 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    noref # 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/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.109E+04 0.128E+04 685. 152. 
;

# 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
Cd1 Cd 0.6667 0.3333 0.3333 0.0168 1.0000 Uani S T . . . .
O2 O 0.8838(3) 0.5391(3) 0.39431(12) 0.0303 1.0000 Uani . . . . . .
C4 C 0.8869(5) 0.6667 0.4167 0.0316 1.0000 Uani S T . . . .
C3 C 0.6667 0.3333 0.0833 0.0253 1.0000 Uani S T . . . .
N5 N 0.8105(5) 0.3333 0.0833 0.0398 1.0000 Uani S T . . . .
H42 H 0.7818 0.6667 0.4167 0.0380 1.0000 Uiso . . . . . .
H52 H 0.8095 0.2404 0.0803 0.0479 1.0000 Uiso . . . . . .
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
Cd1 0.01412(19) 0.01412(19) 0.0222(3) 0.0000 0.0000 0.00706(10)
O2 0.0241(12) 0.0261(12) 0.0426(13) -0.0147(11) -0.0116(10) 0.0140(10)
C4 0.0212(14) 0.035(3) 0.043(3) -0.016(2) -0.0079(11) 0.0176(13)
C3 0.0204(18) 0.0204(18) 0.035(4) 0.0000 0.0000 0.0102(9)
N5 0.0206(14) 0.022(2) 0.078(3) -0.007(2) -0.0037(11) 0.0109(10)

_refine_ls_extinction_coef       59(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          2.03(3)
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
Cd1 . O2 28_545 2.288(2) yes
Cd1 . O2 20_655 2.288(2) yes
Cd1 . O2 21_555 2.288(2) yes
Cd1 . O2 25_665 2.288(2) yes
Cd1 . O2 4_655 2.288(2) yes
Cd1 . O2 . 2.288(2) yes
O2 . C4 . 1.241(3) yes
C4 . H42 . 0.969 no
C3 . N5 33_654 1.325(4) yes
C3 . N5 20_655 1.325(4) yes
C3 . N5 . 1.325(4) yes
N5 . H52 9_554 0.854 no
N5 . H52 . 0.854 no
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
O2 28_545 Cd1 . O2 20_655 84.81(8) yes
O2 28_545 Cd1 . O2 21_555 95.19(8) yes
O2 20_655 Cd1 . O2 21_555 179.995 yes
O2 28_545 Cd1 . O2 25_665 179.995 yes
O2 20_655 Cd1 . O2 25_665 95.19(8) yes
O2 21_555 Cd1 . O2 25_665 84.81(8) yes
O2 28_545 Cd1 . O2 4_655 95.19(8) yes
O2 20_655 Cd1 . O2 4_655 84.81(8) yes
O2 21_555 Cd1 . O2 4_655 95.19(8) yes
O2 25_665 Cd1 . O2 4_655 84.81(8) yes
O2 28_545 Cd1 . O2 . 84.81(8) yes
O2 20_655 Cd1 . O2 . 95.19(8) yes
O2 21_555 Cd1 . O2 . 84.81(8) yes
O2 25_665 Cd1 . O2 . 95.19(8) yes
O2 4_655 Cd1 . O2 . 179.995 yes
Cd1 . O2 . C4 . 124.5(2) yes
O2 . C4 . O2 11_565 126.5(4) yes
O2 . C4 . H42 . 116.8 no
O2 11_565 C4 . H42 . 116.8 no
N5 33_654 C3 . N5 20_655 120.000(3) yes
N5 33_654 C3 . N5 . 120.000(3) yes
N5 20_655 C3 . N5 . 120.000 yes
C3 . N5 . H52 9_554 119.4 no
C3 . N5 . H52 . 119.4 no
H52 9_554 N5 . H52 . 121.2 no
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
N5 . H52 . O2 22_644 172.81 0.854 2.078 2.9279(11) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/11/12 at 17:58:55
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/11/12 at 17:58:55
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_450K
_database_code_depnum_ccdc_archive 'CCDC 1420165'
_audit_update_record             
;
2015-08-21 deposited with the CCDC.
2015-10-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_450K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.48 Ang.
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The  chemistry/geometry is well understood and the hydrogen atoms were refined  with restraints (prior to inclusion in the final refinement using a riding  model) and are within expected parameters.
;
#==============================================================================
# end Validation Reply Form
#==============================================================================

# Added during the CSD deposition process: Friday 21st of August 2015 07:23:07 PM
# end Validation Reply Form

#==============================================================================
_audit_creation_date             12-11-19
_audit_creation_method           CRYSTALS_ver_14.23

_oxford_structure_analysis_title 051iec11
_chemical_name_systematic        'guanidinium cadmium formate'
_chemical_melting_point          'not measured'

_cell_length_a                   9.1803(4)
_cell_length_b                   9.1803(4)
_cell_length_c                   19.8649(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1449.9(2)

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3 c '
_symmetry_space_group_name_Hall  '-R 3 2"c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/3,y+2/3,z+2/3
-x+1/3,-y+2/3,-z+2/3
x+2/3,y+1/3,z+1/3
-x+2/3,-y+1/3,-z+1/3
-y,x-y,z
y,-x+y,-z
-y+1/3,x-y+2/3,z+2/3
y+1/3,-x+y+2/3,-z+2/3
-y+2/3,x-y+1/3,z+1/3
y+2/3,-x+y+1/3,-z+1/3
-x+y,-x,z
x-y,x,-z
-x+y+1/3,-x+2/3,z+2/3
x-y+1/3,x+2/3,-z+2/3
-x+y+2/3,-x+1/3,z+1/3
x-y+2/3,x+1/3,-z+1/3
-x+y,y,z+1/2
x-y,-y,-z+1/2
-x+y+1/3,y+2/3,z+7/6
x-y+1/3,-y+2/3,-z+7/6
-x+y+2/3,y+1/3,z+5/6
x-y+2/3,-y+1/3,-z+5/6
x,x-y,z+1/2
-x,-x+y,-z+1/2
x+1/3,x-y+2/3,z+7/6
-x+1/3,-x+y+2/3,-z+7/6
x+2/3,x-y+1/3,z+5/6
-x+2/3,-x+y+1/3,-z+5/6
-y,-x,z+1/2
y,x,-z+1/2
-y+1/3,-x+2/3,z+7/6
y+1/3,x+2/3,-z+7/6
-y+2/3,-x+1/3,z+5/6
y+2/3,x+1/3,-z+5/6

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'
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'
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'
Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825
5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            6

# Given Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.11 Fooo =    900.00 Mu =     22.70 M =     51.26
# Found Formula = C4 H9 Cd1 N3 O6 
# Dc =      2.11 FOOO =    900.00 Mu =     22.70 M =     51.26

_chemical_formula_sum            'C4 H9 Cd1 N3 O6'
_chemical_formula_moiety         'C3 H3 Cd O6, C H6 N3 '
_chemical_compound_source        'not measured'
_chemical_formula_weight         307.53


_cell_measurement_reflns_used    4917
_cell_measurement_theta_min      3
_cell_measurement_theta_max      31
_cell_measurement_temperature    450

_exptl_crystal_description       lath
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_max          0.20

_exptl_crystal_density_diffrn    2.113
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    2.270

# Sheldrick geometric approximatio 0.71 0.93 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.93
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Refinement of 150 K structure'
_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      450
_diffrn_reflns_number            4399
_reflns_number_total             479
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections with Friedels Law is 479 
# Theoretical number of reflections is about 1011 


_diffrn_reflns_theta_min         3.282
_diffrn_reflns_theta_max         30.820
_diffrn_measured_fraction_theta_max 0.932

_diffrn_reflns_theta_full        26.197
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -11
_reflns_limit_h_max              0
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   1.75
_oxford_diffrn_Wilson_scale      0.30

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

_refine_diff_density_min         -1.05
_refine_diff_density_max         1.13


# 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>-3.0\s(I)
_refine_ls_number_reflns         478
_refine_ls_number_restraints     0
_refine_ls_number_parameters     25
_oxford_refine_ls_R_factor_ref   0.0406
_refine_ls_wR_factor_ref         0.0476
_refine_ls_goodness_of_fit_ref   0.8139
_refine_ls_shift/su_max          0.0000879
_refine_ls_shift/su_mean         0.0000081


# The values computed from all data 
_oxford_reflns_number_all        478
_refine_ls_R_factor_all          0.0406
_refine_ls_wR_factor_all         0.0476

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                357
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_gt          0.0354

# 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    noref # 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/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 936. 935. 560. 92.6 
;

# 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
Cd1 Cd 0.6667 0.3333 0.3333 0.0235 1.0000 Uani S T . . . .
O2 O 0.8832(3) 0.5404(3) 0.39387(13) 0.0435 1.0000 Uani . . . . . .
C4 C 0.8864(5) 0.6667 0.4167 0.0427 1.0000 Uani S T . . . .
C3 C 0.6667 0.3333 0.0833 0.0380 1.0000 Uani S T . . . .
N5 N 0.8096(5) 0.3333 0.0833 0.0575 1.0000 Uani S T . . . .
H42 H 0.7818 0.6667 0.4167 0.0380 1.0000 Uiso . . . . . .
H52 H 0.8095 0.2404 0.0803 0.0479 1.0000 Uiso . . . . . .
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
Cd1 0.0197(2) 0.0197(2) 0.0310(3) 0.0000 0.0000 0.00987(11)
O2 0.0371(14) 0.0373(14) 0.0586(15) -0.0203(13) -0.0158(13) 0.0205(12)
C4 0.0277(16) 0.045(3) 0.061(3) -0.023(3) -0.0114(14) 0.0227(16)
C3 0.029(2) 0.029(2) 0.057(5) 0.0000 0.0000 0.0143(11)
N5 0.0320(18) 0.031(2) 0.109(4) -0.010(3) -0.0052(13) 0.0156(12)

_refine_ls_extinction_coef       76(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          1.97(3)
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
Cd1 . O2 13_665 2.288(2) yes
Cd1 . O2 7_655 2.288(2) yes
Cd1 . O2 16_545 2.288(2) yes
Cd1 . O2 10_555 2.288(2) yes
Cd1 . O2 4_655 2.288(2) yes
Cd1 . O2 . 2.288(2) yes
O2 . C4 . 1.231(3) yes
C4 . H42 . 0.960 no
C3 . N5 34_544 1.313(5) yes
C3 . N5 28_654 1.313(5) yes
C3 . N5 . 1.313(5) yes
N5 . H52 22_554 0.855 no
N5 . H52 . 0.855 no
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
O2 13_665 Cd1 . O2 7_655 94.91(10) yes
O2 13_665 Cd1 . O2 16_545 179.995 yes
O2 7_655 Cd1 . O2 16_545 85.09(10) yes
O2 13_665 Cd1 . O2 10_555 85.09(10) yes
O2 7_655 Cd1 . O2 10_555 179.995 yes
O2 16_545 Cd1 . O2 10_555 94.91(10) yes
O2 13_665 Cd1 . O2 4_655 85.09(10) yes
O2 7_655 Cd1 . O2 4_655 85.09(10) yes
O2 16_545 Cd1 . O2 4_655 94.91(10) yes
O2 10_555 Cd1 . O2 4_655 94.91(10) yes
O2 13_665 Cd1 . O2 . 94.91(10) yes
O2 7_655 Cd1 . O2 . 94.91(10) yes
O2 16_545 Cd1 . O2 . 85.09(10) yes
O2 10_555 Cd1 . O2 . 85.09(10) yes
O2 4_655 Cd1 . O2 . 179.995 yes
Cd1 . O2 . C4 . 125.3(3) yes
O2 24_565 C4 . O2 . 126.9(5) yes
O2 24_565 C4 . H42 . 116.6 no
O2 . C4 . H42 . 116.6 no
N5 34_544 C3 . N5 28_654 120.000 yes
N5 34_544 C3 . N5 . 120.000 yes
N5 28_654 C3 . N5 . 120.000(4) yes
C3 . N5 . H52 22_554 119.9 no
C3 . N5 . H52 . 119.9 no
H52 22_554 N5 . H52 . 120.3 no
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
N5 . H52 . O2 9_644 172.22 0.855 2.085 2.9343(11) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/11/12 at 18:23:29
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/11/12 at 18:23:29
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#==============================================================================
# start Validation Reply Form
#==============================================================================
_vrf_PLAT417_150K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.  
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The 
chemistry/geometry is well understood and the hydrogen atoms were refined 
with restraints (prior to inclusion in the final refinement using a riding 
model) and are within expected parameters.
;
_vrf_PLAT417_250K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.  
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The 
chemistry/geometry is well understood and the hydrogen atoms were refined 
with restraints (prior to inclusion in the final refinement using a riding 
model) and are within expected parameters.
;
_vrf_PLAT417_300K                
;
PROBLEM: Short Inter D-H..H-D       H52    ..  H52     ..       1.49 Ang.  
RESPONSE: This is the H...H distance in the NH2 of the guanidinium.  The 
chemistry/geometry is well understood and the hydrogen atoms were refined 
with restraints (prior to inclusion in the final refinement using a riding 
model) and are within expected parameters.
;
