# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full 'Chemical Science'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_journal_coden_Cambridge 1475
_journal_year 2012
_publ_contact_author 'Andrew L. Goodwin'
_publ_contact_author_email andrew.goodwin@chem.ox.ac.uk
_publ_contact_author_phone '+44 1865 272137'
_contact_author_fax '+44 1865 272690'
loop_
_publ_author_name
_publ_author_address
J.M.Ogborn
;
Department of Chemistry,
University of Oxford,
Inorganic Chemistry Laboratory,
South Parks Road,
Oxford OX1 3QR. UK.
;
I.E.Collings
;
Department of Chemistry,
University of Oxford,
Inorganic Chemistry Laboratory,
South Parks Road,
Oxford OX1 3QR. UK.
;
A.L.Thompson
;
Chemical Crystallography,
Chemistry Research Laboratory,
Department of Chemistry,
University of Oxford,
Mansfield Road,
Oxford OX1 3TA. UK.
;
S.A.Moggach
;
The University of Edinburgh
Joseph Black Building
West Mains Road
Edinburgh
EH9 3JJ
;
A.L.Goodwin
;
Department of Chemistry,
University of Oxford,
Inorganic Chemistry Laboratory,
South Parks Road,
Oxford OX1 3QR. UK.
;
_journal_volume ?
_journal_page_first ?
_journal_page_last ?
_ccdc_journal_depnumber ?
_publ_section_title
;
Supramolecular Mechanics in a Metal-Organic Framework
;
_publ_section_abstract
;
A combination of variable-temperature and variable-pressure
single-crystal and powder X-ray diffraction is used to study
the thermo- and piezo-mechanical properties of the metal-organic
framework (MOF) silver(I) 2-methylimidazolate, Ag(mim). We find
the material to exhibit a number of anomalous mechanical
properties: negative thermal expansion, colossal positive thermal
expansion and the most extreme negative linear compressibility
yet observed for a MOF. By considering the mechanical response
of individual supramolecular motifs we are able to rationalise
the varied and unconventional behaviour of the bulk material.
A general inverse correspondence between strength of supramolecular
interaction and magnitude of mechanical response is identified.
We propose that the consideration of MOF structures in terms of
their underlying mechanical building units provides a straightforward
qualitative method of directing framework design in order to
maximise anomalous mechanical response.
;
_publ_contact_author_name 'Andrew L. Goodwin'
#==============================================================================
data_300K
_database_code_depnum_ccdc_archive 'CCDC 881740'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-05
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 019jmo11
_chemical_name_systematic .
_chemical_melting_point 'not measured'
_cell_length_a 7.8946(6)
_cell_length_b 5.9692(4)
_cell_length_c 10.8812(10)
_cell_angle_alpha 90
_cell_angle_beta 92.454(3)
_cell_angle_gamma 90
_cell_volume 512.30(7)
_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'
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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C3 H6 Ag0.25 N0.25 O3
# Dc = 1.56 Fooo = 360.00 Mu = 10.39 M = 120.55
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.45 FOOO = 360.00 Mu = 37.86 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source .
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 1106
_cell_measurement_theta_min 3
_cell_measurement_theta_max 27
_cell_measurement_temperature 300
_exptl_crystal_description plate
_exptl_crystal_colour clear_pale_colourless
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 2.450
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.786
# Sheldrick geometric approximatio 0.68 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min 0.85
_exptl_absorpt_correction_T_max 0.89
# 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 \w
# 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 known model'
_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 4050
_reflns_number_total 1174
_diffrn_reflns_av_R_equivalents 0.027
# Number of reflections without Friedels Law is 2023
# Number of reflections with Friedels Law is 1174
# Theoretical number of reflections is about 1179
_diffrn_reflns_theta_min 3.125
_diffrn_reflns_theta_max 27.514
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 26.963
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.44
_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 1169
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0728
_refine_ls_wR_factor_ref 0.0735
_refine_ls_goodness_of_fit_ref 1.0241
_refine_ls_shift/su_max 0.0000499
_refine_ls_shift/su_mean 0.0000072
# The values computed from all data
_oxford_reflns_number_all 1169
_refine_ls_R_factor_all 0.0728
_refine_ls_wR_factor_all 0.0735
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 631
_refine_ls_R_factor_gt 0.0302
_refine_ls_wR_factor_gt 0.0466
# 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:
5.84 7.15 2.02
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
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.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0364 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0391 1.0000 Uani S . . . . .
C1 C 0.3806(11) 0.9500(15) 0.6846(8) 0.0468 1.0000 Uani . . . . . .
C2 C 0.4797(8) 0.7634(12) 0.7444(6) 0.0237 1.0000 Uani . . . . . .
C3 C 0.6194(9) 0.4535(13) 0.7728(6) 0.0320 1.0000 Uani . . . . . .
C4 C 0.6155(10) 0.5588(13) 0.8805(6) 0.0371 1.0000 Uani . . . . . .
N1 N 0.5320(7) 0.5817(10) 0.6841(4) 0.0281 1.0000 Uani . . . . . .
N2 N 0.5286(8) 0.7588(10) 0.8653(5) 0.0296 1.0000 Uani . . . . . .
H13 H 0.3919 1.0817 0.7334 0.0699 1.0000 Uiso R . . . . .
H12 H 0.4197 0.9807 0.6051 0.0699 1.0000 Uiso R . . . . .
H11 H 0.2647 0.9090 0.6778 0.0701 1.0000 Uiso R . . . . .
H31 H 0.6722 0.3164 0.7587 0.0381 1.0000 Uiso R . . . . .
H41 H 0.6645 0.5086 0.9540 0.0439 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
Ag1 0.0562(5) 0.0358(5) 0.0172(4) -0.0100(3) 0.0027(3) -0.0037(4)
Ag2 0.0576(6) 0.0390(5) 0.0210(4) -0.0143(3) 0.0059(3) -0.0042(4)
C1 0.050(5) 0.043(5) 0.047(4) 0.001(4) -0.004(4) 0.004(4)
C2 0.031(3) 0.022(3) 0.018(3) -0.005(2) 0.003(2) -0.003(3)
C3 0.031(4) 0.034(4) 0.030(3) -0.002(3) 0.000(3) 0.000(3)
C4 0.049(4) 0.038(4) 0.024(3) 0.004(3) 0.000(3) -0.002(4)
N1 0.035(3) 0.032(3) 0.017(2) -0.010(2) 0.002(2) -0.001(3)
N2 0.040(3) 0.033(3) 0.016(2) -0.005(2) 0.005(2) -0.002(3)
_refine_ls_extinction_coef 7.9(6)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 0.2522(4)
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
Ag1 . N1 2_666 2.067(5) yes
Ag1 . N1 . 2.067(5) yes
Ag2 . N2 2_677 2.074(5) yes
Ag2 . N2 . 2.074(5) yes
C1 . C2 . 1.494(10) yes
C1 . H13 . 0.951 no
C1 . H12 . 0.949 no
C1 . H11 . 0.947 no
C2 . N1 . 1.342(8) yes
C2 . N2 . 1.356(8) yes
C3 . C4 . 1.332(9) yes
C3 . N1 . 1.391(8) yes
C3 . H31 . 0.934 no
C4 . N2 . 1.383(10) yes
C4 . H41 . 0.924 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 109.8 no
C2 . C1 . H12 . 110.9 no
H13 . C1 . H12 . 108.8 no
C2 . C1 . H11 . 109.1 no
H13 . C1 . H11 . 109.0 no
H12 . C1 . H11 . 109.2 no
C1 . C2 . N1 . 123.8(6) yes
C1 . C2 . N2 . 124.0(7) yes
N1 . C2 . N2 . 112.2(6) yes
C4 . C3 . N1 . 108.7(6) yes
C4 . C3 . H31 . 125.8 no
N1 . C3 . H31 . 125.4 no
C3 . C4 . N2 . 109.4(6) yes
C3 . C4 . H41 . 125.8 no
N2 . C4 . H41 . 124.8 no
C3 . N1 . C2 . 105.0(5) yes
C3 . N1 . Ag1 . 125.4(4) yes
C2 . N1 . Ag1 . 129.6(5) yes
C4 . N2 . C2 . 104.6(6) yes
C4 . N2 . Ag2 . 125.7(4) yes
C2 . N2 . Ag2 . 129.6(5) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/01/12 at 15:46:05
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/01/12 at 15:46:05
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 1 0 x .
_chemical_name_common .
#==============================================================================
data_250K
_database_code_depnum_ccdc_archive 'CCDC 881741'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-05
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 016jmo11
_chemical_name_systematic .
_chemical_melting_point 'not measured'
_cell_length_a 7.8401(6)
_cell_length_b 5.9549(4)
_cell_length_c 10.8935(10)
_cell_angle_alpha 90
_cell_angle_beta 92.556(3)
_cell_angle_gamma 90
_cell_volume 508.08(7)
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 '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'
_cell_formula_units_Z 4
# Given Formula = C4 H5 Ag1 N2
# Dc = 2.47 Fooo = 360.00 Mu = 38.17 M = 188.97
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.47 FOOO = 360.00 Mu = 38.17 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source .
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 1090
_cell_measurement_theta_min 1
_cell_measurement_theta_max 27
_cell_measurement_temperature 250
_exptl_crystal_description plate
_exptl_crystal_colour clear_pale_colourless
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 2.470
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.817
# Sheldrick geometric approximatio 0.68 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min 0.85
_exptl_absorpt_correction_T_max 0.89
# 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 \w
# 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 known model'
_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 3941
_reflns_number_total 1162
_diffrn_reflns_av_R_equivalents 0.023
# Number of reflections without Friedels Law is 1996
# Number of reflections with Friedels Law is 1162
# Theoretical number of reflections is about 1170
_diffrn_reflns_theta_min 3.136
_diffrn_reflns_theta_max 27.522
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 25.320
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 14
_oxford_diffrn_Wilson_B_factor 2.15
_oxford_diffrn_Wilson_scale 17.85
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.17
_refine_diff_density_max 1.20
# 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 1157
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0673
_refine_ls_wR_factor_ref 0.0699
_refine_ls_goodness_of_fit_ref 1.0417
_refine_ls_shift/su_max 0.0000526
_refine_ls_shift/su_mean 0.0000045
# The values computed from all data
_oxford_reflns_number_all 1157
_refine_ls_R_factor_all 0.0673
_refine_ls_wR_factor_all 0.0699
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 641
_refine_ls_R_factor_gt 0.0284
_refine_ls_wR_factor_gt 0.0463
# 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:
5.94 7.22 2.09
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
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.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0301 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0319 1.0000 Uani S . . . . .
C1 C 0.3801(9) 0.9487(14) 0.6848(7) 0.0352 1.0000 Uani . . . . . .
C2 C 0.4813(9) 0.7643(13) 0.7447(6) 0.0234 1.0000 Uani . . . . . .
C3 C 0.6190(9) 0.4520(12) 0.7720(6) 0.0273 1.0000 Uani . . . . . .
C4 C 0.6144(9) 0.5577(13) 0.8808(6) 0.0285 1.0000 Uani . . . . . .
N1 N 0.5320(7) 0.5806(9) 0.6842(5) 0.0241 1.0000 Uani . . . . . .
N2 N 0.5284(7) 0.7580(10) 0.8640(5) 0.0269 1.0000 Uani . . . . . .
H13 H 0.3831 1.0782 0.7363 0.0528 1.0000 Uiso R . . . . .
H12 H 0.4273 0.9857 0.6080 0.0531 1.0000 Uiso R . . . . .
H11 H 0.2652 0.9000 0.6712 0.0532 1.0000 Uiso R . . . . .
H31 H 0.6716 0.3149 0.7580 0.0331 1.0000 Uiso R . . . . .
H41 H 0.6619 0.5059 0.9546 0.0340 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
Ag1 0.0455(5) 0.0302(5) 0.0148(3) -0.0083(3) 0.0026(3) -0.0025(4)
Ag2 0.0473(5) 0.0312(5) 0.0176(4) -0.0112(3) 0.0053(3) -0.0034(4)
C1 0.034(4) 0.031(4) 0.041(4) -0.003(4) 0.002(3) 0.004(3)
C2 0.027(3) 0.027(3) 0.016(3) -0.008(2) 0.002(2) 0.002(3)
C3 0.033(4) 0.023(3) 0.027(3) -0.002(3) 0.006(3) 0.003(3)
C4 0.033(4) 0.034(4) 0.019(3) 0.001(3) 0.001(2) 0.006(3)
N1 0.031(3) 0.025(3) 0.016(2) -0.007(2) 0.002(2) 0.001(3)
N2 0.032(3) 0.029(3) 0.020(3) -0.005(2) 0.002(2) -0.002(3)
_refine_ls_extinction_coef 7.5(6)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 0.2531(4)
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
Ag1 . N1 2_666 2.068(5) yes
Ag1 . N1 . 2.068(5) yes
Ag2 . N2 2_677 2.086(6) yes
Ag2 . N2 . 2.086(6) yes
C1 . C2 . 1.488(10) yes
C1 . H13 . 0.953 no
C1 . H12 . 0.955 no
C1 . H11 . 0.952 no
C2 . N1 . 1.346(9) yes
C2 . N2 . 1.336(8) yes
C3 . C4 . 1.343(9) yes
C3 . N1 . 1.381(8) yes
C3 . H31 . 0.930 no
C4 . N2 . 1.378(9) yes
C4 . H41 . 0.924 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 109.9 no
C2 . C1 . H12 . 109.6 no
H13 . C1 . H12 . 109.2 no
C2 . C1 . H11 . 109.0 no
H13 . C1 . H11 . 109.7 no
H12 . C1 . H11 . 109.5 no
C1 . C2 . N1 . 123.3(6) yes
C1 . C2 . N2 . 124.5(7) yes
N1 . C2 . N2 . 112.2(6) yes
C4 . C3 . N1 . 108.6(6) yes
C4 . C3 . H31 . 125.8 no
N1 . C3 . H31 . 125.6 no
C3 . C4 . N2 . 108.7(6) yes
C3 . C4 . H41 . 125.8 no
N2 . C4 . H41 . 125.4 no
C3 . N1 . C2 . 105.0(5) yes
C3 . N1 . Ag1 . 125.3(4) yes
C2 . N1 . Ag1 . 129.6(5) yes
C4 . N2 . C2 . 105.4(6) yes
C4 . N2 . Ag2 . 124.8(4) yes
C2 . N2 . Ag2 . 129.6(5) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/01/12 at 16:11:11
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/01/12 at 16:11:11
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 1 0 x .
_chemical_name_common .
#==============================================================================
data_200K
_database_code_depnum_ccdc_archive 'CCDC 881742'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-05
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 017jmo11
_chemical_name_systematic .
_chemical_melting_point 'not measured'
_cell_length_a 7.7899(6)
_cell_length_b 5.9402(4)
_cell_length_c 10.9075(10)
_cell_angle_alpha 90
_cell_angle_beta 92.670(3)
_cell_angle_gamma 90
_cell_volume 504.18(7)
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 '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'
_cell_formula_units_Z 4
# Given Formula = C4 H5 Ag1 N2
# Dc = 2.49 Fooo = 360.00 Mu = 38.46 M = 188.97
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.49 FOOO = 360.00 Mu = 38.46 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source .
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 1084
_cell_measurement_theta_min 3
_cell_measurement_theta_max 27
_cell_measurement_temperature 200
_exptl_crystal_description plate
_exptl_crystal_colour clear_pale_colourless
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 2.489
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.846
# Sheldrick geometric approximatio 0.68 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min 0.84
_exptl_absorpt_correction_T_max 0.89
# 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 \w
# 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 known model'
_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 200
_diffrn_reflns_number 3980
_reflns_number_total 1147
_diffrn_reflns_av_R_equivalents 0.022
# Number of reflections without Friedels Law is 1989
# Number of reflections with Friedels Law is 1147
# Theoretical number of reflections is about 1158
_diffrn_reflns_theta_min 3.145
_diffrn_reflns_theta_max 27.502
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full 25.302
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 14
_oxford_diffrn_Wilson_B_factor 1.84
_oxford_diffrn_Wilson_scale 17.21
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.20
_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 1143
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0615
_refine_ls_wR_factor_ref 0.0843
_refine_ls_goodness_of_fit_ref 1.0074
_refine_ls_shift/su_max 0.0000438
_refine_ls_shift/su_mean 0.0000077
# The values computed from all data
_oxford_reflns_number_all 1143
_refine_ls_R_factor_all 0.0615
_refine_ls_wR_factor_all 0.0843
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 626
_refine_ls_R_factor_gt 0.0253
_refine_ls_wR_factor_gt 0.0538
# 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:
9.30 13.4 6.58 1.73
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
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.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0248 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0262 1.0000 Uani S . . . . .
C1 C 0.3775(9) 0.9503(12) 0.6848(6) 0.0308 1.0000 Uani . . . . . .
C2 C 0.4794(7) 0.7644(11) 0.7440(5) 0.0211 1.0000 Uani . . . . . .
C3 C 0.6171(7) 0.4491(12) 0.7719(5) 0.0252 1.0000 Uani . . . . . .
C4 C 0.6141(8) 0.5569(12) 0.8806(5) 0.0274 1.0000 Uani . . . . . .
N1 N 0.5313(6) 0.5800(9) 0.6848(4) 0.0198 1.0000 Uani . . . . . .
N2 N 0.5288(7) 0.7573(10) 0.8647(4) 0.0230 1.0000 Uani . . . . . .
H13 H 0.3760 1.0765 0.7379 0.0447 1.0000 Uiso R . . . . .
H12 H 0.4273 0.9939 0.6107 0.0448 1.0000 Uiso R . . . . .
H11 H 0.2632 0.8997 0.6667 0.0454 1.0000 Uiso R . . . . .
H31 H 0.6685 0.3118 0.7575 0.0290 1.0000 Uiso R . . . . .
H41 H 0.6621 0.5038 0.9540 0.0319 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
Ag1 0.0368(4) 0.0247(4) 0.0129(3) -0.0066(2) 0.0018(2) -0.0013(3)
Ag2 0.0386(4) 0.0257(4) 0.0147(3) -0.0088(2) 0.0039(2) -0.0021(3)
C1 0.038(4) 0.023(3) 0.032(3) 0.000(3) 0.002(3) 0.003(3)
C2 0.025(3) 0.025(3) 0.014(2) -0.004(2) 0.003(2) -0.010(3)
C3 0.022(3) 0.027(3) 0.027(3) 0.004(3) 0.005(2) 0.003(3)
C4 0.031(3) 0.033(4) 0.017(3) 0.004(3) -0.003(2) 0.001(3)
N1 0.024(2) 0.023(2) 0.013(2) -0.006(2) 0.0027(17) 0.005(2)
N2 0.030(3) 0.026(3) 0.012(2) -0.0046(19) 0.0022(18) -0.003(2)
_refine_ls_extinction_coef 9.9(10)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 0.2555(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
Ag1 . N1 2_666 2.074(4) yes
Ag1 . N1 . 2.074(4) yes
Ag2 . N2 2_677 2.083(5) yes
Ag2 . N2 . 2.083(5) yes
C1 . C2 . 1.490(9) yes
C1 . H13 . 0.947 no
C1 . H12 . 0.948 no
C1 . H11 . 0.952 no
C2 . N1 . 1.344(8) yes
C2 . N2 . 1.355(6) yes
C3 . C4 . 1.348(8) yes
C3 . N1 . 1.377(7) yes
C3 . H31 . 0.925 no
C4 . N2 . 1.371(9) yes
C4 . H41 . 0.924 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 110.0 no
C2 . C1 . H12 . 109.9 no
H13 . C1 . H12 . 108.8 no
C2 . C1 . H11 . 109.3 no
H13 . C1 . H11 . 109.8 no
H12 . C1 . H11 . 109.0 no
C1 . C2 . N1 . 124.2(5) yes
C1 . C2 . N2 . 124.5(6) yes
N1 . C2 . N2 . 111.3(6) yes
C4 . C3 . N1 . 108.1(6) yes
C4 . C3 . H31 . 126.4 no
N1 . C3 . H31 . 125.5 no
C3 . C4 . N2 . 109.2(5) yes
C3 . C4 . H41 . 125.3 no
N2 . C4 . H41 . 125.5 no
C3 . N1 . C2 . 106.0(5) yes
C3 . N1 . Ag1 . 124.9(4) yes
C2 . N1 . Ag1 . 129.0(4) yes
C4 . N2 . C2 . 105.3(5) yes
C4 . N2 . Ag2 . 125.4(4) yes
C2 . N2 . Ag2 . 129.2(5) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/01/12 at 16:26:53
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/01/12 at 16:26:53
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
_chemical_name_common .
#==============================================================================
data_150K
_database_code_depnum_ccdc_archive 'CCDC 881743'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-05
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 018jmo11
_chemical_name_systematic .
_chemical_melting_point .
_cell_length_a 7.7378(6)
_cell_length_b 5.9245(4)
_cell_length_c 10.9232(9)
_cell_angle_alpha 90
_cell_angle_beta 92.821(3)
_cell_angle_gamma 90
_cell_volume 500.14(7)
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 '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'
_cell_formula_units_Z 4
# Given Formula = C4 H5 Ag1 N2
# Dc = 2.51 Fooo = 360.00 Mu = 38.78 M = 188.97
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.51 FOOO = 360.00 Mu = 38.78 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source .
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 1094
_cell_measurement_theta_min 3
_cell_measurement_theta_max 27
_cell_measurement_temperature 150
_exptl_crystal_description plate
_exptl_crystal_colour clear_pale_colourless
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 2.509
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.878
# Sheldrick geometric approximatio 0.68 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min 0.85
_exptl_absorpt_correction_T_max 0.89
# 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 \w
# 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 known model'
_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 3972
_reflns_number_total 1126
_diffrn_reflns_av_R_equivalents 0.023
# Number of reflections without Friedels Law is 1980
# Number of reflections with Friedels Law is 1126
# Theoretical number of reflections is about 1136
_diffrn_reflns_theta_min 3.154
_diffrn_reflns_theta_max 27.387
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 26.839
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_reflns_limit_h_min -9
_reflns_limit_h_max 9
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 14
_oxford_diffrn_Wilson_B_factor 1.51
_oxford_diffrn_Wilson_scale 16.97
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.39
_refine_diff_density_max 1.18
# 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 1122
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0562
_refine_ls_wR_factor_ref 0.0642
_refine_ls_goodness_of_fit_ref 1.0290
_refine_ls_shift/su_max 0.0000627
_refine_ls_shift/su_mean 0.0000115
# The values computed from all data
_oxford_reflns_number_all 1122
_refine_ls_R_factor_all 0.0562
_refine_ls_wR_factor_all 0.0642
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 640
_refine_ls_R_factor_gt 0.0256
_refine_ls_wR_factor_gt 0.0418
# 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:
6.30 7.76 2.17
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
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.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0183 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0193 1.0000 Uani S . . . . .
C1 C 0.3782(8) 0.9537(11) 0.6869(6) 0.0224 1.0000 Uani . . . . . .
C2 C 0.4790(7) 0.7625(11) 0.7447(5) 0.0156 1.0000 Uani . . . . . .
C3 C 0.6161(7) 0.4467(11) 0.7714(5) 0.0198 1.0000 Uani . . . . . .
C4 C 0.6147(7) 0.5569(11) 0.8806(5) 0.0204 1.0000 Uani . . . . . .
N1 N 0.5316(6) 0.5793(8) 0.6841(4) 0.0166 1.0000 Uani . . . . . .
N2 N 0.5270(6) 0.7585(9) 0.8645(4) 0.0178 1.0000 Uani . . . . . .
H13 H 0.3805 1.0823 0.7396 0.0341 1.0000 Uiso R . . . . .
H12 H 0.4265 0.9962 0.6122 0.0338 1.0000 Uiso R . . . . .
H11 H 0.2606 0.9096 0.6693 0.0342 1.0000 Uiso R . . . . .
H31 H 0.6668 0.3072 0.7577 0.0238 1.0000 Uiso R . . . . .
H41 H 0.6649 0.5056 0.9541 0.0247 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
Ag1 0.0270(4) 0.0179(3) 0.0100(3) -0.0045(2) 0.0016(2) -0.0013(3)
Ag2 0.0291(4) 0.0186(4) 0.0104(3) -0.0062(2) 0.0034(2) -0.0017(3)
C1 0.025(3) 0.017(3) 0.026(3) 0.002(3) -0.002(2) 0.000(3)
C2 0.016(3) 0.016(3) 0.015(2) -0.003(2) 0.006(2) -0.005(2)
C3 0.021(3) 0.018(3) 0.022(3) -0.002(2) 0.002(2) 0.005(2)
C4 0.019(3) 0.025(3) 0.017(3) 0.003(3) -0.003(2) 0.000(3)
N1 0.019(2) 0.018(2) 0.013(2) -0.0039(19) 0.0021(18) 0.002(2)
N2 0.021(2) 0.024(3) 0.009(2) -0.005(2) 0.0018(17) 0.001(2)
_refine_ls_extinction_coef 7.2(6)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 0.2502(4)
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
Ag1 . N1 2_666 2.068(4) yes
Ag1 . N1 . 2.068(4) yes
Ag2 . N2 2_677 2.077(5) yes
Ag2 . N2 . 2.077(5) yes
C1 . C2 . 1.497(8) yes
C1 . H13 . 0.955 no
C1 . H12 . 0.949 no
C1 . H11 . 0.957 no
C2 . N1 . 1.345(8) yes
C2 . N2 . 1.343(7) yes
C3 . C4 . 1.360(8) yes
C3 . N1 . 1.376(7) yes
C3 . H31 . 0.930 no
C4 . N2 . 1.381(8) yes
C4 . H41 . 0.926 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 110.8 no
C2 . C1 . H12 . 110.1 no
H13 . C1 . H12 . 108.1 no
C2 . C1 . H11 . 110.4 no
H13 . C1 . H11 . 109.2 no
H12 . C1 . H11 . 108.1 no
C1 . C2 . N1 . 124.6(5) yes
C1 . C2 . N2 . 122.5(5) yes
N1 . C2 . N2 . 112.9(5) yes
C4 . C3 . N1 . 108.0(5) yes
C4 . C3 . H31 . 126.1 no
N1 . C3 . H31 . 125.8 no
C3 . C4 . N2 . 109.2(5) yes
C3 . C4 . H41 . 125.6 no
N2 . C4 . H41 . 125.3 no
C3 . N1 . C2 . 105.4(5) yes
C3 . N1 . Ag1 . 125.0(4) yes
C2 . N1 . Ag1 . 129.6(4) yes
C4 . N2 . C2 . 104.5(5) yes
C4 . N2 . Ag2 . 124.8(4) yes
C2 . N2 . Ag2 . 130.5(4) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/01/12 at 16:57:01
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/01/12 at 16:57:01
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
_chemical_name_common .
#==============================================================================
data_100K
_database_code_depnum_ccdc_archive 'CCDC 881744'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-05
_audit_creation_method CRYSTALS_ver_14.23
_oxford_structure_analysis_title 019jmo11
_chemical_name_systematic .
_chemical_melting_point 'not measured'
_cell_length_a 7.6885(6)
_cell_length_b 5.9097(4)
_cell_length_c 10.9351(9)
_cell_angle_alpha 90
_cell_angle_beta 92.984(3)
_cell_angle_gamma 90
_cell_volume 496.18(7)
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 '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'
_cell_formula_units_Z 4
# Given Formula = C4 H5 Ag1 N2
# Dc = 2.53 Fooo = 360.00 Mu = 39.09 M = 188.97
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.53 FOOO = 360.00 Mu = 39.09 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source .
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 1092
_cell_measurement_theta_min 3
_cell_measurement_theta_max 27
_cell_measurement_temperature 100
_exptl_crystal_description plate
_exptl_crystal_colour clear_pale_colourless
_exptl_crystal_size_min 0.030
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.120
_exptl_crystal_density_diffrn 2.529
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.909
# Sheldrick geometric approximatio 0.68 0.89
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min 0.83
_exptl_absorpt_correction_T_max 0.89
# 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 \w
# 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 known model'
_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 3937
_reflns_number_total 1135
_diffrn_reflns_av_R_equivalents 0.022
# Number of reflections without Friedels Law is 1990
# Number of reflections with Friedels Law is 1135
# Theoretical number of reflections is about 1149
_diffrn_reflns_theta_min 3.163
_diffrn_reflns_theta_max 27.579
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 26.752
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_reflns_limit_h_min -9
_reflns_limit_h_max 9
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 14
_oxford_diffrn_Wilson_B_factor 1.13
_oxford_diffrn_Wilson_scale 16.86
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.08
_refine_diff_density_max 1.35
# 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 1131
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0547
_refine_ls_wR_factor_ref 0.0636
_refine_ls_goodness_of_fit_ref 1.0166
_refine_ls_shift/su_max 0.0000526
_refine_ls_shift/su_mean 0.0000082
# The values computed from all data
_oxford_reflns_number_all 1131
_refine_ls_R_factor_all 0.0547
_refine_ls_wR_factor_all 0.0636
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 654
_refine_ls_R_factor_gt 0.0251
_refine_ls_wR_factor_gt 0.0438
# 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:
6.83 8.48 2.45
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
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.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0126 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0134 1.0000 Uani S . . . . .
C1 C 0.3769(7) 0.9516(11) 0.6857(5) 0.0168 1.0000 Uani . . . . . .
C2 C 0.4804(7) 0.7623(11) 0.7446(5) 0.0125 1.0000 Uani . . . . . .
C3 C 0.6180(7) 0.4447(10) 0.7715(5) 0.0129 1.0000 Uani . . . . . .
C4 C 0.6159(7) 0.5552(11) 0.8812(5) 0.0161 1.0000 Uani . . . . . .
N1 N 0.5304(6) 0.5788(8) 0.6840(4) 0.0132 1.0000 Uani . . . . . .
N2 N 0.5272(6) 0.7563(9) 0.8649(4) 0.0142 1.0000 Uani . . . . . .
H13 H 0.3818 1.0811 0.7385 0.0251 1.0000 Uiso R . . . . .
H12 H 0.4239 0.9917 0.6104 0.0245 1.0000 Uiso R . . . . .
H11 H 0.2579 0.9062 0.6709 0.0250 1.0000 Uiso R . . . . .
H31 H 0.6690 0.3048 0.7566 0.0160 1.0000 Uiso R . . . . .
H41 H 0.6650 0.5026 0.9544 0.0189 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
Ag1 0.0187(3) 0.0123(3) 0.0070(3) -0.0031(2) 0.0013(2) -0.0004(2)
Ag2 0.0193(3) 0.0130(3) 0.0080(3) -0.0041(2) 0.0020(2) -0.0011(2)
C1 0.015(3) 0.018(3) 0.017(3) 0.002(3) -0.001(2) 0.002(2)
C2 0.015(3) 0.013(3) 0.009(2) 0.000(2) 0.0033(19) -0.002(2)
C3 0.013(3) 0.011(3) 0.014(3) 0.000(2) -0.001(2) 0.003(2)
C4 0.015(3) 0.023(3) 0.010(2) 0.005(2) 0.0007(19) -0.002(2)
N1 0.016(2) 0.013(2) 0.011(2) -0.0034(18) -0.0018(17) 0.001(2)
N2 0.017(2) 0.016(2) 0.009(2) -0.0041(19) 0.0001(17) 0.003(2)
_refine_ls_extinction_coef 6.2(5)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 0.2484(4)
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
Ag1 . N1 2_666 2.067(4) yes
Ag1 . N1 . 2.067(4) yes
Ag2 . N2 2_677 2.082(5) yes
Ag2 . N2 . 2.082(5) yes
C1 . C2 . 1.499(8) yes
C1 . H13 . 0.959 no
C1 . H12 . 0.947 no
C1 . H11 . 0.959 no
C2 . N1 . 1.338(8) yes
C2 . N2 . 1.345(7) yes
C3 . C4 . 1.367(8) yes
C3 . N1 . 1.389(7) yes
C3 . H31 . 0.933 no
C4 . N2 . 1.377(8) yes
C4 . H41 . 0.921 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 109.5 no
C2 . C1 . H12 . 110.0 no
H13 . C1 . H12 . 108.6 no
C2 . C1 . H11 . 110.1 no
H13 . C1 . H11 . 109.4 no
H12 . C1 . H11 . 109.1 no
C1 . C2 . N1 . 123.5(5) yes
C1 . C2 . N2 . 123.2(5) yes
N1 . C2 . N2 . 113.2(5) yes
C4 . C3 . N1 . 107.7(5) yes
C4 . C3 . H31 . 126.9 no
N1 . C3 . H31 . 125.4 no
C3 . C4 . N2 . 109.0(5) yes
C3 . C4 . H41 . 125.3 no
N2 . C4 . H41 . 125.6 no
C3 . N1 . C2 . 105.2(4) yes
C3 . N1 . Ag1 . 124.6(4) yes
C2 . N1 . Ag1 . 130.1(4) yes
C4 . N2 . C2 . 104.8(5) yes
C4 . N2 . Ag2 . 124.9(4) yes
C2 . N2 . Ag2 . 130.1(4) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/01/12 at 17:04:58
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/01/12 at 17:04:58
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
_chemical_name_common .
#==============================================================================
data_0.0GPa
_database_code_depnum_ccdc_archive 'CCDC 881745'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-05-11
_audit_creation_method CRYSTALS_ver_14.21
_oxford_structure_analysis_title 'ST1020 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C5 H5 Ag0.25 N1
# Dc = 1.37 Fooo = 360.00 Mu = 9.91 M = 106.07
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.45 FOOO = 360.00 Mu = 37.84 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure '101.325 '
_publ_section_exptl_refinement
;
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.02
This is caused by the methyl group on the imidazole ligand, which
shows slightly larger thermal motion due to its greater
flexibility than those atoms within the ring. The principal axes of
the thermal elipsoids however are all very reasonable for room
temperature data;
Principal axes of the thermal ellipsoids, A**2
Min Med Max Uarith Ugeom Uprime
AG 1. 0.0123 0.0408 0.0542 0.0358 0.0301 0.1795
AG 2. 0.0124 0.0442 0.0589 0.0385 0.0318 0.2103
C 1. 0.0358 0.0388 0.0540 0.0429 0.0422 0.0585
C 2. 0.0164 0.0288 0.0355 0.0269 0.0256 0.0626
C 3. 0.0263 0.0329 0.0357 0.0316 0.0314 0.0448
C 4. 0.0237 0.0379 0.0393 0.0337 0.0328 0.0630
N 1. 0.0148 0.0312 0.0384 0.0281 0.0261 0.0810
N 2. 0.0144 0.0329 0.0397 0.0290 0.0266 0.0907
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 7
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 76
The data are complete.
#==============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
#==============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#------------------------------------------------------------------------------
20.82 0.500 0.998 531 530 1
23.01 0.550 0.999 715 714 1
25.24 0.600 0.999 929 928 1
#----------------------------------------------------------- ACTA Min. Res. ---
27.51 0.650 0.998 1178 1176 2
29.43 0.691 0.946 1417 1340 77
128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
This was chosen as to get a beta angle closer to 90 degrees.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 7.8926(5)
_cell_length_b 5.9767(3)
_cell_length_c 10.8739(6)
_cell_angle_alpha 90
_cell_angle_beta 92.470(5)
_cell_angle_gamma 90
_cell_volume 512.46(5)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 3476
_cell_measurement_theta_min 3
_cell_measurement_theta_max 29
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 2.449
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 3.784
# Sheldrick geometric approximatio 0.47 0.68
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.46
_exptl_absorpt_correction_T_max 0.68
_diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)'
_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_reflns_number 9493
_reflns_number_total 1341
_diffrn_reflns_av_R_equivalents 0.024
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 1341
# Theoretical number of reflections is about 2837
_diffrn_reflns_theta_min 3.126
_diffrn_reflns_theta_max 29.431
_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full 25.605
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 14
_reflns_limit_h_min -10
_reflns_limit_h_max 10
_reflns_limit_k_min 0
_reflns_limit_k_max 8
_reflns_limit_l_min 0
_reflns_limit_l_max 14
_oxford_diffrn_Wilson_B_factor 2.56
_oxford_diffrn_Wilson_scale 0.01
_atom_sites_solution_primary Direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.64
_refine_diff_density_max 0.64
# 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 1340
_refine_ls_number_restraints 0
_refine_ls_number_parameters 68
_oxford_refine_ls_R_factor_ref 0.0379
_refine_ls_wR_factor_ref 0.0681
_refine_ls_goodness_of_fit_ref 1.0721
_refine_ls_shift/su_max 0.0004978
_refine_ls_shift/su_mean 0.0000832
# The values computed from all data
_oxford_reflns_number_all 1340
_refine_ls_R_factor_all 0.0379
_refine_ls_wR_factor_all 0.0681
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 1026
_refine_ls_R_factor_gt 0.0248
_refine_ls_wR_factor_gt 0.0602
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 0.52P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Sheldrick, G. M. (2008). Acta Cryst A64, 112-122.
Oxford Diffraction, (2010). CrysAlisPro.
Oxford Diffraction, (2002). Xcalibur 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.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0358 1.0000 Uani S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0385 1.0000 Uani S . . . . .
C1 C 0.3799(5) 0.9478(6) 0.6858(3) 0.0429 1.0000 Uani . . . . . .
C2 C 0.4799(3) 0.7640(4) 0.7447(2) 0.0269 1.0000 Uani . . . . . .
C3 C 0.6173(4) 0.4523(5) 0.7713(3) 0.0316 1.0000 Uani . . . . . .
C4 C 0.6149(4) 0.5600(5) 0.8805(3) 0.0337 1.0000 Uani . . . . . .
N1 N 0.5320(3) 0.5813(4) 0.68473(19) 0.0281 1.0000 Uani . . . . . .
N2 N 0.5279(3) 0.7582(4) 0.86418(19) 0.0290 1.0000 Uani . . . . . .
H13 H 0.2676 0.9033 0.6662 0.0685 1.0000 Uiso R . . . . .
H12 H 0.4294 0.9947 0.6106 0.0682 1.0000 Uiso R . . . . .
H11 H 0.3773 1.0759 0.7393 0.0673 1.0000 Uiso R . . . . .
H31 H 0.6693 0.3118 0.7571 0.0401 1.0000 Uiso R . . . . .
H41 H 0.6646 0.5070 0.9561 0.0433 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
Ag1 0.0533(3) 0.0364(2) 0.01769(19) -0.01138(11) 0.00231(14) -0.00360(13)
Ag2 0.0560(3) 0.0386(2) 0.0213(2) -0.01510(12) 0.00630(15) -0.00454(14)
C1 0.048(2) 0.0396(17) 0.0402(19) -0.0041(15) -0.0037(15) 0.0046(16)
C2 0.0324(14) 0.0290(14) 0.0194(13) -0.0062(11) 0.0022(11) -0.0033(12)
C3 0.0334(16) 0.0307(14) 0.0311(16) -0.0034(12) 0.0044(12) 0.0009(12)
C4 0.0375(17) 0.0382(16) 0.0249(14) 0.0004(13) -0.0030(12) -0.0004(14)
N1 0.0312(12) 0.0327(13) 0.0204(11) -0.0100(10) 0.0012(9) 0.0006(11)
N2 0.0371(13) 0.0322(13) 0.0178(10) -0.0077(9) 0.0031(9) -0.0029(10)
_refine_ls_extinction_coef 14.8(13)
_refine_ls_extinction_method 'Larson (1970), Equation 22'
_oxford_refine_ls_scale 5.37(17)
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
Ag1 . N1 2_666 2.072(2) yes
Ag1 . N1 . 2.072(2) yes
Ag2 . N2 2_677 2.085(2) yes
Ag2 . N2 . 2.085(2) yes
C1 . C2 . 1.482(4) yes
C1 . H13 . 0.941 no
C1 . H12 . 0.963 no
C1 . H11 . 0.961 no
C2 . N1 . 1.345(3) yes
C2 . N2 . 1.338(3) yes
C3 . C4 . 1.351(4) yes
C3 . N1 . 1.371(4) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.377(4) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H13 . 111.5 no
C2 . C1 . H12 . 110.8 no
H13 . C1 . H12 . 107.5 no
C2 . C1 . H11 . 110.7 no
H13 . C1 . H11 . 108.6 no
H12 . C1 . H11 . 107.6 no
C1 . C2 . N1 . 124.1(2) yes
C1 . C2 . N2 . 124.2(2) yes
N1 . C2 . N2 . 111.7(2) yes
C4 . C3 . N1 . 108.1(3) yes
C4 . C3 . H31 . 125.9 no
N1 . C3 . H31 . 126.0 no
C3 . C4 . N2 . 108.8(3) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.7 no
C3 . N1 . C2 . 105.9(2) yes
C3 . N1 . Ag1 . 124.74(19) yes
C2 . N1 . Ag1 . 129.30(19) yes
C4 . N2 . C2 . 105.4(2) yes
C4 . N2 . Ag2 . 124.92(18) yes
C2 . N2 . Ag2 . 129.49(19) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 11/05/11 at 09:21:19
#
#LIST 12
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 11/05/11 at 09:21:19
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-6 2 12 x .
#==============================================================================
data_1.1GPa
_database_code_depnum_ccdc_archive 'CCDC 881746'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-05-19
_audit_creation_method CRYSTALS_ver_14.21
_oxford_structure_analysis_title 'st1025 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag1 N2
# Dc = 2.50 Fooo = 360.00 Mu = 41.16 M = 176.95
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.67 FOOO = 360.00 Mu = 41.25 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure '1 100 000 '
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.36
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 17.38 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.38
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.17 Deg.
342_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 25
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.554 57
088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.57
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5
950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6
These are all caused by shading of the pressure cell.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
This has been placed geometrically.
731_ALERT_1_C Bond Calc 1.48(3), Rep 1.481(9) ...... 3.33 su-Ra
C1 -C2 1.555 1.555
731_ALERT_1_C Bond Calc 1.35(2), Rep 1.355(9) ...... 2.22 su-Ra
C3 -C4 1.555 1.555
731_ALERT_1_C Bond Calc 1.368(19), Rep 1.369(9) ...... 2.11 su-Ra
C3 -N1 1.555 1.555
731_ALERT_1_C Bond Calc 1.38(2), Rep 1.378(9) ...... 2.22 su-Ra
C4 -N2 1.555 1.555
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 7.433(2)
_cell_length_b 5.8092(3)
_cell_length_c 10.9101(5)
_cell_angle_alpha 90
_cell_angle_beta 93.736(10)
_cell_angle_gamma 90
_cell_volume 470.09(13)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 518
_cell_measurement_theta_min 4
_cell_measurement_theta_max 26
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 2.670
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.125
# Sheldrick geometric approximatio 0.44 0.66
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.43
_exptl_absorpt_correction_T_max 0.66
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 1222
_reflns_number_total 241
_diffrn_reflns_av_R_equivalents 0.033
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 241
# Theoretical number of reflections is about 1337
_diffrn_reflns_theta_min 3.743
_diffrn_reflns_theta_max 23.175
_diffrn_measured_fraction_theta_max 0.357
_diffrn_reflns_theta_full 17.381
_diffrn_measured_fraction_theta_full 0.378
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 12
_reflns_limit_h_min -2
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 6
_reflns_limit_l_min 0
_reflns_limit_l_max 12
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.54
_refine_diff_density_max 1.34
# 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 240
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.1072
_refine_ls_wR_factor_ref 0.2123
_refine_ls_goodness_of_fit_ref 1.1132
_refine_ls_shift/su_max 0.0019476
_refine_ls_shift/su_mean 0.0003112
# The values computed from all data
_oxford_reflns_number_all 240
_refine_ls_R_factor_all 0.1072
_refine_ls_wR_factor_all 0.2123
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 151
_refine_ls_R_factor_gt 0.0821
_refine_ls_wR_factor_gt 0.2029
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +41.61P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
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.
;
# 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
Ag1 Ag 0.5000 0.5000 0.5000 0.0202(13) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0234(14) 1.0000 Uiso S . . . . .
C1 C 0.376(7) 0.951(4) 0.682(2) 0.013(3) 1.0000 Uiso D U . . . .
C2 C 0.4804(15) 0.762(2) 0.7434(12) 0.013(3) 1.0000 Uiso D U . . . .
C3 C 0.6173(15) 0.435(2) 0.7731(16) 0.012(3) 1.0000 Uiso D U . . . .
C4 C 0.6157(15) 0.547(3) 0.8818(13) 0.012(3) 1.0000 Uiso D U . . . .
N1 N 0.5312(16) 0.571(2) 0.6853(12) 0.013(3) 1.0000 Uiso D U . . . .
N2 N 0.5290(16) 0.755(2) 0.8635(12) 0.012(3) 1.0000 Uiso D U . . . .
H11 H 0.3552 1.0683 0.7404 0.0153 1.0000 Uiso R . . . . .
H12 H 0.4422 1.0136 0.6183 0.0153 1.0000 Uiso R . . . . .
H13 H 0.2639 0.8938 0.6485 0.0153 1.0000 Uiso R . . . . .
H31 H 0.6689 0.2878 0.7602 0.0150 1.0000 Uiso R . . . . .
H41 H 0.6663 0.4917 0.9584 0.0150 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1742(9)
loop_
_oxford_twin_element_scale_factors
0.67(2)
0.33(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
Ag1 . N1 2_666 2.061(13) yes
Ag1 . N1 . 2.061(13) yes
Ag2 . N2 2_677 2.080(13) yes
Ag2 . N2 . 2.080(13) yes
C1 . C2 . 1.481(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.344(9) yes
C2 . N2 . 1.337(9) yes
C3 . C4 . 1.355(9) yes
C3 . N1 . 1.369(9) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.378(9) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.8(7) yes
C1 . C2 . N2 . 124.3(7) yes
N1 . C2 . N2 . 111.9(6) yes
C4 . C3 . N1 . 107.7(6) yes
C4 . C3 . H31 . 126.2 no
N1 . C3 . H31 . 126.2 no
C3 . C4 . N2 . 109.1(6) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.5 no
C3 . N1 . C2 . 106.2(6) yes
C3 . N1 . Ag1 . 126.1(9) yes
C2 . N1 . Ag1 . 127.6(9) yes
C4 . N2 . C2 . 105.1(6) yes
C4 . N2 . Ag2 . 124.4(9) yes
C2 . N2 . Ag2 . 130.4(9) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/05/11 at 11:17:59
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/05/11 at 11:17:59
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-2 1 5 x .
#==============================================================================
data_2.2GPa
_database_code_depnum_ccdc_archive 'CCDC 881747'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-05-19
_audit_creation_method CRYSTALS_ver_14.21
_oxford_structure_analysis_title 'st1026 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag1 N2
# Dc = 2.64 Fooo = 360.00 Mu = 43.40 M = 176.95
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.82 FOOO = 360.00 Mu = 43.50 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure '2 200 000 '
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.32
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.33
342_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 23
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 63
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 10
950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6
These are all caused by shading of the pressure cell.
084_ALERT_2_C High R2 Value .................................. 0.26
The sample is weakly diffracting, causing the high value of R2.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
731_ALERT_1_C Bond Calc 1.48(3), Rep 1.482(9) ...... 3.33 su-Ra
C1 -C2 1.555 1.55
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 7.2027(16)
_cell_length_b 5.6926(3)
_cell_length_c 10.9057(4)
_cell_angle_alpha 90
_cell_angle_beta 94.504(8)
_cell_angle_gamma 90
_cell_volume 445.78(10)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 699
_cell_measurement_theta_min 4
_cell_measurement_theta_max 26
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 2.815
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.350
# Sheldrick geometric approximatio 0.42 0.65
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.43
_exptl_absorpt_correction_T_max 0.65
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 1631
_reflns_number_total 295
_diffrn_reflns_av_R_equivalents 0.025
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 295
# Theoretical number of reflections is about 1821
_diffrn_reflns_theta_min 3.748
_diffrn_reflns_theta_max 26.362
_diffrn_measured_fraction_theta_max 0.323
_diffrn_reflns_theta_full 25.044
_diffrn_measured_fraction_theta_full 0.329
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -2
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.30
_refine_diff_density_max 1.32
# 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 295
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.1055
_refine_ls_wR_factor_ref 0.2574
_refine_ls_goodness_of_fit_ref 1.0632
_refine_ls_shift/su_max 0.0012710
_refine_ls_shift/su_mean 0.0002000
# The values computed from all data
_oxford_reflns_number_all 295
_refine_ls_R_factor_all 0.1055
_refine_ls_wR_factor_all 0.2574
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 198
_refine_ls_R_factor_gt 0.0891
_refine_ls_wR_factor_gt 0.2447
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.10P)^2^ +32.31P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
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.
;
# 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
Ag1 Ag 0.5000 0.5000 0.5000 0.0193(11) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0215(11) 1.0000 Uiso S . . . . .
C1 C 0.372(5) 0.946(3) 0.6820(15) 0.015(3) 1.0000 Uiso D U . . . .
C2 C 0.4779(15) 0.751(2) 0.7443(9) 0.015(2) 1.0000 Uiso D U . . . .
C3 C 0.6264(15) 0.423(2) 0.7740(12) 0.015(2) 1.0000 Uiso D U . . . .
C4 C 0.6224(15) 0.535(2) 0.8833(11) 0.015(2) 1.0000 Uiso D U . . . .
N1 N 0.5344(16) 0.560(2) 0.6857(10) 0.015(2) 1.0000 Uiso D U . . . .
N2 N 0.5282(16) 0.744(2) 0.8652(10) 0.015(2) 1.0000 Uiso D U . . . .
H11 H 0.3488 1.0652 0.7400 0.0156 1.0000 Uiso R . . . . .
H12 H 0.4472 1.0081 0.6220 0.0156 1.0000 Uiso R . . . . .
H13 H 0.2569 0.8932 0.6430 0.0156 1.0000 Uiso R . . . . .
H31 H 0.6786 0.2723 0.7614 0.0150 1.0000 Uiso R . . . . .
H41 H 0.6756 0.4777 0.9601 0.0149 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1766(10)
loop_
_oxford_twin_element_scale_factors
0.73(2)
0.27(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
Ag1 . N1 2_666 2.049(10) yes
Ag1 . N1 . 2.049(10) yes
Ag2 . N2 2_677 2.091(11) yes
Ag2 . N2 . 2.091(11) yes
C1 . C2 . 1.482(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.343(9) yes
C2 . N2 . 1.340(9) yes
C3 . C4 . 1.354(9) yes
C3 . N1 . 1.369(9) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.378(9) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.995 yes
C2 . C1 . H11 . 109.9 no
C2 . C1 . H12 . 106.9 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 111.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.6(7) yes
C1 . C2 . N2 . 124.3(7) yes
N1 . C2 . N2 . 112.1(6) yes
C4 . C3 . N1 . 108.0(6) yes
C4 . C3 . H31 . 126.0 no
N1 . C3 . H31 . 126.0 no
C3 . C4 . N2 . 109.0(6) yes
C3 . C4 . H41 . 125.4 no
N2 . C4 . H41 . 125.6 no
C3 . N1 . C2 . 106.0(6) yes
C3 . N1 . Ag1 . 128.0(8) yes
C2 . N1 . Ag1 . 126.0(8) yes
C4 . N2 . C2 . 105.0(6) yes
C4 . N2 . Ag2 . 125.1(8) yes
C2 . N2 . Ag2 . 129.6(7) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/05/11 at 11:21:04
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/05/11 at 11:21:04
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
#==============================================================================
data_3.3GPa
_database_code_depnum_ccdc_archive 'CCDC 881748'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-05-19
_audit_creation_method CRYSTALS_ver_14.21
_oxford_structure_analysis_title 'st1027 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag2 N2
# Dc = 4.41 Fooo = 360.00 Mu = 89.56 M = 284.82
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.93 FOOO = 360.00 Mu = 45.25 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure '3 300 000 '
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.31
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 72
342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 19
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 16
950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6
These are all caused by shading of the pressure cell.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
060_ALERT_4_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.25
Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. Here, residual absorption errors from the pressure
cell are an obvious source of further systematic error.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
The methyl group was placed geometrically and could not be refined.
731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2.22 su-Ra
C1 -C2 1.555 1.555
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 7.0544(17)
_cell_length_b 5.6024(3)
_cell_length_c 10.8873(4)
_cell_angle_alpha 90
_cell_angle_beta 95.062(9)
_cell_angle_gamma 90
_cell_volume 428.61(11)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 569
_cell_measurement_theta_min 4
_cell_measurement_theta_max 26
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 2.928
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.525
# Sheldrick geometric approximatio 0.40 0.64
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.53
_exptl_absorpt_correction_T_max 0.64
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 283
_reflns_number_total 283
_diffrn_reflns_av_R_equivalents 0.021
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 283
# Theoretical number of reflections is about 1835
_diffrn_reflns_theta_min 3.758
_diffrn_reflns_theta_max 26.809
_diffrn_measured_fraction_theta_max 0.308
_diffrn_reflns_theta_full 25.201
_diffrn_measured_fraction_theta_full 0.318
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -2
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.58
_refine_diff_density_max 1.34
# 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 283
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.0996
_refine_ls_wR_factor_ref 0.1910
_refine_ls_goodness_of_fit_ref 1.0400
_refine_ls_shift/su_max 0.0017690
_refine_ls_shift/su_mean 0.0002787
# The values computed from all data
_oxford_reflns_number_all 283
_refine_ls_R_factor_all 0.0996
_refine_ls_wR_factor_all 0.1910
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 174
_refine_ls_R_factor_gt 0.0728
_refine_ls_wR_factor_gt 0.1758
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +28.97P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
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.
;
# 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
Ag1 Ag 0.5000 0.5000 0.5000 0.0162(8) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0178(8) 1.0000 Uiso S . . . . .
C1 C 0.380(5) 0.948(3) 0.6799(14) 0.011(2) 1.0000 Uiso D U . . . .
C2 C 0.4868(14) 0.750(2) 0.7439(9) 0.011(2) 1.0000 Uiso D U . . . .
C3 C 0.6249(15) 0.408(2) 0.7771(12) 0.011(2) 1.0000 Uiso D U . . . .
C4 C 0.6265(15) 0.527(2) 0.8852(10) 0.011(2) 1.0000 Uiso D U . . . .
N1 N 0.5364(15) 0.550(2) 0.6870(9) 0.011(2) 1.0000 Uiso D U . . . .
N2 N 0.5387(15) 0.745(2) 0.8649(9) 0.011(2) 1.0000 Uiso D U . . . .
H11 H 0.3606 1.0714 0.7374 0.0146 1.0000 Uiso R . . . . .
H12 H 0.4501 1.0085 0.6163 0.0146 1.0000 Uiso R . . . . .
H13 H 0.2598 0.8911 0.6452 0.0146 1.0000 Uiso R . . . . .
H31 H 0.6757 0.2531 0.7656 0.0137 1.0000 Uiso R . . . . .
H41 H 0.6799 0.4692 0.9627 0.0136 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1789(7)
loop_
_oxford_twin_element_scale_factors
0.788(19)
0.212(19)
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
Ag1 . N1 2_666 2.048(10) yes
Ag1 . N1 . 2.048(10) yes
Ag2 . N2 2_677 2.086(10) yes
Ag2 . N2 . 2.086(10) yes
C1 . C2 . 1.480(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.345(8) yes
C2 . N2 . 1.336(8) yes
C3 . C4 . 1.352(9) yes
C3 . N1 . 1.370(9) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.379(9) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.4 no
C2 . C1 . H12 . 109.4 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.5(6) yes
C1 . C2 . N2 . 124.3(6) yes
N1 . C2 . N2 . 112.1(6) yes
C4 . C3 . N1 . 107.8(6) yes
C4 . C3 . H31 . 126.2 no
N1 . C3 . H31 . 126.0 no
C3 . C4 . N2 . 109.2(6) yes
C3 . C4 . H41 . 125.3 no
N2 . C4 . H41 . 125.5 no
C3 . N1 . C2 . 106.0(6) yes
C3 . N1 . Ag1 . 130.0(8) yes
C2 . N1 . Ag1 . 123.8(7) yes
C4 . N2 . C2 . 104.9(6) yes
C4 . N2 . Ag2 . 125.4(7) yes
C2 . N2 . Ag2 . 129.7(7) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/05/11 at 11:23:04
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/05/11 at 11:23:04
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
#==============================================================================
data_3.8GPa
_database_code_depnum_ccdc_archive 'CCDC 881749'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-05-19
_audit_creation_method CRYSTALS_ver_14.21
_oxford_structure_analysis_title 'st1028 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag2 N2
# Dc = 4.49 Fooo = 360.00 Mu = 91.21 M = 284.82
# Found Formula = C4 H5 Ag1 N2
# Dc = 2.98 FOOO = 360.00 Mu = 46.08 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure '3 800 000 '
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.31
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 71
342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 18
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 3
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 16
950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 6
These are all caused by shading of the pressure cell.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
413_ALERT_2_B Short Inter XH3 .. XHn H13 .. H41 .. 2.08 Ang.
Short contacts are expected at high pressure.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
060_ALERT_4_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.14
Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc. Here, residual absorption errors from the pressure
cell are an obvious source of further systematic error.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
The methyl group was placed geometrically and could not be refined.
731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2.22 su-Ra
C1 -C2 1.555 1.555
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
128_ALERT_4_G Non-standard setting of Space-group P21/c .... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 3
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 6.9920(13)
_cell_length_b 5.5590(2)
_cell_length_c 10.8750(4)
_cell_angle_alpha 90
_cell_angle_beta 95.344(7)
_cell_angle_gamma 90
_cell_volume 420.86(8)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 704
_cell_measurement_theta_min 4
_cell_measurement_theta_max 27
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 2.982
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.608
# Sheldrick geometric approximatio 0.40 0.63
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.47
_exptl_absorpt_correction_T_max 0.63
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 281
_reflns_number_total 281
_diffrn_reflns_av_R_equivalents 0.019
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 281
# Theoretical number of reflections is about 1817
_diffrn_reflns_theta_min 3.764
_diffrn_reflns_theta_max 26.889
_diffrn_measured_fraction_theta_max 0.309
_diffrn_reflns_theta_full 25.007
_diffrn_measured_fraction_theta_full 0.321
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -2
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 1.04
_oxford_diffrn_Wilson_scale 84.51
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.62
_refine_diff_density_max 1.23
# 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 280
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.0954
_refine_ls_wR_factor_ref 0.2066
_refine_ls_goodness_of_fit_ref 0.9796
_refine_ls_shift/su_max 0.0016779
_refine_ls_shift/su_mean 0.0002653
# The values computed from all data
_oxford_reflns_number_all 280
_refine_ls_R_factor_all 0.0954
_refine_ls_wR_factor_all 0.2066
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 188
_refine_ls_R_factor_gt 0.0772
_refine_ls_wR_factor_gt 0.1932
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +36.79P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
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.
;
# 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
Ag1 Ag 0.5000 0.5000 0.5000 0.0153(9) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0166(9) 1.0000 Uiso S . . . . .
C1 C 0.381(6) 0.951(3) 0.6789(15) 0.013(2) 1.0000 Uiso D U . . . .
C2 C 0.4794(14) 0.7454(18) 0.7443(9) 0.012(2) 1.0000 Uiso D U . . . .
C3 C 0.6219(15) 0.4024(19) 0.7776(11) 0.012(2) 1.0000 Uiso D U . . . .
C4 C 0.6276(15) 0.524(2) 0.8854(10) 0.012(2) 1.0000 Uiso D U . . . .
N1 N 0.5283(15) 0.543(2) 0.6875(9) 0.012(2) 1.0000 Uiso D U . . . .
N2 N 0.5371(15) 0.7431(19) 0.8650(9) 0.012(2) 1.0000 Uiso D U . . . .
H11 H 0.3601 1.0743 0.7365 0.0147 1.0000 Uiso R . . . . .
H12 H 0.4580 1.0105 0.6185 0.0147 1.0000 Uiso R . . . . .
H13 H 0.2605 0.8987 0.6398 0.0147 1.0000 Uiso R . . . . .
H31 H 0.6733 0.2466 0.7663 0.0139 1.0000 Uiso R . . . . .
H41 H 0.6846 0.4684 0.9629 0.0140 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1734(8)
loop_
_oxford_twin_element_scale_factors
0.80(2)
0.20(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
Ag1 . N1 2_666 2.044(10) yes
Ag1 . N1 . 2.044(10) yes
Ag2 . N2 2_677 2.081(10) yes
Ag2 . N2 . 2.081(10) yes
C1 . C2 . 1.480(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.344(8) yes
C2 . N2 . 1.337(8) yes
C3 . C4 . 1.352(9) yes
C3 . N1 . 1.371(9) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.379(9) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.4 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.5(6) yes
C1 . C2 . N2 . 124.3(6) yes
N1 . C2 . N2 . 112.2(6) yes
C4 . C3 . N1 . 107.9(6) yes
C4 . C3 . H31 . 126.0 no
N1 . C3 . H31 . 126.1 no
C3 . C4 . N2 . 109.1(6) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.4 no
C3 . N1 . C2 . 105.9(6) yes
C3 . N1 . Ag1 . 129.9(8) yes
C2 . N1 . Ag1 . 123.5(7) yes
C4 . N2 . C2 . 105.0(6) yes
C4 . N2 . Ag2 . 125.2(7) yes
C2 . N2 . Ag2 . 129.8(7) 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
C1 . H11 . C2 3_556 121.1(6) 0.950 2.583 3.18(2) yes
C3 . H31 . C3 3_646 165.2(4) 0.950 2.463 3.39(2) yes
C3 . H31 . C4 3_646 139.0(4) 0.950 2.572 3.35(2) yes
C3 . H31 . N1 3_646 137.7(4) 0.950 2.386 3.15(2) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/05/11 at 11:24:28
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/05/11 at 11:24:28
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
2 4 4 x .
#==============================================================================
data_4.9GPa
_database_code_depnum_ccdc_archive 'CCDC 881750'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-08-08
_audit_creation_method CRYSTALS_ver_14.11
_oxford_structure_analysis_title 'st1031 in P2(1)/n'
_chemical_name_systematic ?
_chemical_melting_point ?
_publ_section_exptl_refinement
;
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.335
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 73
088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.89
342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 18
950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 6
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1
These are all caused by shading of the pressure cell.
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
413_ALERT_2_C Short Inter XH3 .. XHn H13 .. H41 .. 2.11 Ang.
Short contacts are expected at high pressure.
731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2 su-Ra
C1 -C2 1.555 1.555
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1
These are correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
929_ALERT_5_G No Weight Pars,Obs and Calc R1,wR2,S not checked !
No action taken.
808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found !
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 6.9259(16)
_cell_length_b 5.5072(2)
_cell_length_c 10.8549(4)
_cell_angle_alpha 90
_cell_angle_beta 95.667(8)
_cell_angle_gamma 90
_cell_volume 412.01(10)
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C3 H5 Ag2 N2
# Dc = 4.59 Fooo = 360.00 Mu = 93.17 M = 284.82
# Found Formula = C4 H5 Ag1 N2
# Dc = 3.05 FOOO = 360.00 Mu = 47.07 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_formula_moiety 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 545
_cell_measurement_theta_min 4
_cell_measurement_theta_max 27
_cell_measurement_temperature 293
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 3.046
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.707
# Sheldrick geometric approximatio 0.39 0.62
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.46
_exptl_absorpt_correction_T_max 0.62
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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 293
_diffrn_reflns_number 277
_reflns_number_total 277
_diffrn_reflns_av_R_equivalents 0.021
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 277
# Theoretical number of reflections is about 1825
_diffrn_reflns_theta_min 3.773
_diffrn_reflns_theta_max 27.141
_diffrn_measured_fraction_theta_max 0.304
_diffrn_reflns_theta_full 25.241
_diffrn_measured_fraction_theta_full 0.335
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -2
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_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 geom
_refine_diff_density_min -1.47
_refine_diff_density_max 1.40
# 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 277
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.1020
_refine_ls_wR_factor_ref 0.2048
_refine_ls_goodness_of_fit_ref 1.0542
_refine_ls_shift/su_max 0.0054769
_refine_ls_shift/su_mean 0.0007388
# The values computed from all data
_oxford_reflns_number_all 277
_refine_ls_R_factor_all 0.1020
_refine_ls_wR_factor_all 0.2048
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 175
_refine_ls_R_factor_gt 0.0751
_refine_ls_wR_factor_gt 0.1891
# 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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +21.17P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0161(8) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0169(9) 1.0000 Uiso S . . . . .
C1 C 0.374(5) 0.946(3) 0.6786(13) 0.014(2) 1.0000 Uiso D U . . . .
C2 C 0.4812(14) 0.7442(18) 0.7443(8) 0.013(2) 1.0000 Uiso D U . . . .
C3 C 0.6238(15) 0.3972(19) 0.7792(11) 0.012(2) 1.0000 Uiso D U . . . .
C4 C 0.6296(15) 0.522(2) 0.8867(10) 0.013(2) 1.0000 Uiso D U . . . .
N1 N 0.5296(15) 0.5388(19) 0.6886(9) 0.013(2) 1.0000 Uiso D U . . . .
N2 N 0.5392(15) 0.7430(19) 0.8652(9) 0.013(2) 1.0000 Uiso D U . . . .
H11 H 0.3561 1.0734 0.7355 0.0184 1.0000 Uiso R . . . . .
H12 H 0.4453 1.0058 0.6145 0.0184 1.0000 Uiso R . . . . .
H13 H 0.2515 0.8885 0.6439 0.0184 1.0000 Uiso R . . . . .
H31 H 0.6752 0.2395 0.7686 0.0172 1.0000 Uiso R . . . . .
H41 H 0.6858 0.4654 0.9649 0.0177 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1716(8)
loop_
_oxford_twin_element_scale_factors
0.87(2)
0.13(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
Ag1 . N1 2_666 2.049(9) yes
Ag1 . N1 . 2.049(9) yes
Ag2 . N2 2_677 2.073(10) yes
Ag2 . N2 . 2.073(10) yes
C1 . C2 . 1.480(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.341(8) yes
C2 . N2 . 1.334(8) yes
C3 . C4 . 1.351(8) yes
C3 . N1 . 1.369(9) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.379(9) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.4 no
C2 . C1 . H12 . 110.0 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.0 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.5(6) yes
C1 . C2 . N2 . 124.5(6) yes
N1 . C2 . N2 . 112.0(6) yes
C4 . C3 . N1 . 107.7(6) yes
C4 . C3 . H31 . 126.1 no
N1 . C3 . H31 . 126.3 no
C3 . C4 . N2 . 109.1(6) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.4 no
C3 . N1 . C2 . 106.2(6) yes
C3 . N1 . Ag1 . 130.7(7) yes
C2 . N1 . Ag1 . 122.3(6) yes
C4 . N2 . C2 . 105.0(6) yes
C4 . N2 . Ag2 . 124.9(7) yes
C2 . N2 . Ag2 . 130.0(7) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 08/08/11 at 15:28:52
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 08/08/11 at 15:28:52
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
#==============================================================================
data_5.6GPa
_database_code_depnum_ccdc_archive 'CCDC 881751'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 11-08-08
_audit_creation_method CRYSTALS_ver_14.11
_oxford_structure_analysis_title 'st1033 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag2 N2
# Dc = 4.67 Fooo = 360.00 Mu = 94.78 M = 284.82
# Found Formula = C4 H5 Ag1 N2
# Dc = 3.10 FOOO = 360.00 Mu = 47.88 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure ' 5 600 000 '
_publ_section_exptl_refinement
;
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.337
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 186
088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.64
342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 16
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 43
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 3
950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 5
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 2
These are all caused by shading and absorption from the pressure cell.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
413_ALERT_2_B Short Inter XH3 .. XHn H13 .. H41 .. 2.05 Ang.
Short contacts are expected at high pressure.
731_ALERT_1_C Bond Calc 1.48(2), Rep 1.480(9) ...... 2 su-Ra
C1 -C2 1.555 1.555 # 5
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1
This has been alerted because the Ag-atoms have been pushed closer together
at high pressure (see text).
128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
This is correct.
380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
The methyl group was placed geometrically and could not be refined.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found !
A shelx weighting scheme was not used.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 6.8710(13)
_cell_length_b 5.4670(2)
_cell_length_c 10.8393(3)
_cell_angle_alpha 90
_cell_angle_beta 95.878(7)
_cell_angle_gamma 90
_cell_volume 405.02(8)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 648
_cell_measurement_theta_min 4
_cell_measurement_theta_max 26
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 3.099
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.788
# Sheldrick geometric approximatio 0.38 0.62
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.48
_exptl_absorpt_correction_T_max 0.62
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 1488
_reflns_number_total 270
_diffrn_reflns_av_R_equivalents 0.028
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 270
# Theoretical number of reflections is about 1795
_diffrn_reflns_theta_min 3.779
_diffrn_reflns_theta_max 27.142
_diffrn_measured_fraction_theta_max 0.302
_diffrn_reflns_theta_full 25.243
_diffrn_measured_fraction_theta_full 0.337
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_h_max 2
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -3
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 7
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_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 geom
_refine_diff_density_min -1.23
_refine_diff_density_max 1.29
# 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 270
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.0753
_refine_ls_wR_factor_ref 0.1595
_refine_ls_goodness_of_fit_ref 1.0147
_refine_ls_shift/su_max 0.0018230
_refine_ls_shift/su_mean 0.0002636
# The values computed from all data
_oxford_reflns_number_all 270
_refine_ls_R_factor_all 0.0753
_refine_ls_wR_factor_all 0.1595
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 192
_refine_ls_R_factor_gt 0.0601
_refine_ls_wR_factor_gt 0.1492
_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= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.07P)^2^ +23.28P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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
Ag1 Ag 0.5000 0.5000 0.5000 0.0138(7) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0143(7) 1.0000 Uiso S . . . . .
C1 C 0.373(5) 0.946(3) 0.6777(12) 0.013(2) 1.0000 Uiso D U . . . .
C2 C 0.4753(14) 0.7395(15) 0.7445(8) 0.0120(17) 1.0000 Uiso D U . . . .
C3 C 0.6215(15) 0.3919(17) 0.7795(9) 0.0117(18) 1.0000 Uiso D U . . . .
C4 C 0.6288(15) 0.5176(19) 0.8874(8) 0.0116(18) 1.0000 Uiso D U . . . .
N1 N 0.5239(15) 0.5328(16) 0.6887(7) 0.0119(17) 1.0000 Uiso D U . . . .
N2 N 0.5362(15) 0.7398(16) 0.8658(8) 0.0112(17) 1.0000 Uiso D U . . . .
H11 H 0.3529 1.0732 0.7347 0.0151 1.0000 Uiso R . . . . .
H12 H 0.4503 1.0055 0.6164 0.0151 1.0000 Uiso R . . . . .
H13 H 0.2501 0.8920 0.6390 0.0151 1.0000 Uiso R . . . . .
H31 H 0.6746 0.2339 0.7686 0.0141 1.0000 Uiso R . . . . .
H41 H 0.6881 0.4619 0.9654 0.0140 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1879(7)
loop_
_oxford_twin_element_scale_factors
0.892(18)
0.108(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
Ag1 . N1 2_666 2.043(8) yes
Ag1 . N1 . 2.043(8) yes
Ag2 . N2 2_677 2.068(8) yes
Ag2 . N2 . 2.068(8) yes
C1 . C2 . 1.480(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.340(8) yes
C2 . N2 . 1.338(8) yes
C3 . C4 . 1.353(8) yes
C3 . N1 . 1.370(8) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.380(8) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.4 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.6 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.4(6) yes
C1 . C2 . N2 . 124.4(6) yes
N1 . C2 . N2 . 112.2(5) yes
C4 . C3 . N1 . 107.9(6) yes
C4 . C3 . H31 . 126.0 no
N1 . C3 . H31 . 126.0 no
C3 . C4 . N2 . 109.0(6) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.5 no
C3 . N1 . C2 . 106.1(5) yes
C3 . N1 . Ag1 . 130.8(6) yes
C2 . N1 . Ag1 . 121.8(6) yes
C4 . N2 . C2 . 104.9(5) yes
C4 . N2 . Ag2 . 124.9(6) yes
C2 . N2 . Ag2 . 130.1(6) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 08/08/11 at 15:41:10
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 08/08/11 at 15:41:10
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
#==============================================================================
data_6.4GPa
_database_code_depnum_ccdc_archive 'CCDC 881752'
#TrackingRef '- CrystallographicData.cif'
#==============================================================================
_audit_creation_date 12-01-19
_audit_creation_method CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'st1034 in P2(1)/n'
_chemical_name_systematic ?
_chemical_formula_moiety 'C4 H5 Ag1 N2'
# Given Formula = C3 H5 Ag2 N2
# Dc = 4.74 Fooo = 360.00 Mu = 96.23 M = 284.82
# Found Formula = C4 H5 Ag1 N2
# Dc = 3.15 FOOO = 360.00 Mu = 48.61 M = 188.97
_chemical_formula_sum 'C4 H5 Ag1 N2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure ' 6 400 000 '
_publ_section_exptl_refinement
;
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.32
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.600 186
088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.50
342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 16
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2
912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 36
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 2
950_ALERT_5_G Reported and Calculated Hmax Values Differ by .. 5
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) .. 1
These are all caused by shading and absorption from the pressure cell.
201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 8
210_ALERT_3_B No Anisotropic ADP's Found in CIF .............. ?
This refinement strategy was based on the low completeness of the data,
which meant that non-H atoms could only be refined with isotropic
thermal parameters.
413_ALERT_2_C Short Inter XH3 .. XHn H13 .. H41 .. 2.12 Ang.
Short contacts are expected at high pressure.
731_ALERT_1_C Bond Calc 1.48(2), Rep 1.479(9) ...... 2 su-Ra
C1 -C2 1.555 1.555 # 5
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif is badly in error.
004_ALERT_5_G Info: Polymeric Structure Found with Dimension . 1
This has been alerted because the Ag-atoms have been pushed closer together
at high pressure (see text).
128_ALERT_4_G Alternate Setting of Space-group P21/c ....... P21/n
This has been chosen to have a beta angle closer to 90 degrees, and therefore
reduce correlation between positional parameters.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature 293 K
This is correct.
380_ALERT_4_G Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1
The methyl group was placed geometrically and could not be refined.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
808_ALERT_5_G No Parseable SHELXL Style Weighting Scheme Found !
A shelx weighting scheme was not used.
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 31
All 1,2 and 1,3 distances were restrained to ambient pressure values
(see text).
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 6.828(2)
_cell_length_b 5.4298(3)
_cell_length_c 10.8209(5)
_cell_angle_alpha 90
_cell_angle_beta 96.076(11)
_cell_angle_gamma 90
_cell_volume 398.92(12)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
_symmetry_int_tables_number 14
# 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 .
_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'
Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156
5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 188.97
_cell_measurement_reflns_used 569
_cell_measurement_theta_min 4
_cell_measurement_theta_max 27
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 3.146
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 360
_exptl_absorpt_coefficient_mu 4.861
# Sheldrick geometric approximatio 0.38 0.61
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.35
_exptl_absorpt_correction_T_max 0.61
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION'
_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_reflns_number 1463
_reflns_number_total 266
_diffrn_reflns_av_R_equivalents 0.040
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 266
# Theoretical number of reflections is about 1702
_diffrn_reflns_theta_min 3.787
_diffrn_reflns_theta_max 26.773
_diffrn_measured_fraction_theta_max 0.312
_diffrn_reflns_theta_full 25.167
_diffrn_measured_fraction_theta_full 0.324
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_h_max 3
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -3
_reflns_limit_h_max 2
_reflns_limit_k_min 0
_reflns_limit_k_max 6
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.47
_refine_diff_density_max 1.69
# 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 266
_refine_ls_number_restraints 31
_refine_ls_number_parameters 28
_oxford_refine_ls_R_factor_ref 0.0820
_refine_ls_wR_factor_ref 0.1545
_refine_ls_goodness_of_fit_ref 1.0033
_refine_ls_shift/su_max 0.0040945
_refine_ls_shift/su_mean 0.0006928
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 266
_refine_ls_R_factor_all 0.0820
_refine_ls_wR_factor_all 0.1545
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 177
_refine_ls_R_factor_gt 0.0615
_refine_ls_wR_factor_gt 0.1410
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +30.29P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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 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
Ag1 Ag 0.5000 0.5000 0.5000 0.0114(7) 1.0000 Uiso S . . . . .
Ag2 Ag 0.5000 1.0000 1.0000 0.0125(7) 1.0000 Uiso S . . . . .
C1 C 0.371(5) 0.941(3) 0.6776(12) 0.010(2) 1.0000 Uiso D U . . . .
C2 C 0.4826(14) 0.7390(16) 0.7441(8) 0.0100(17) 1.0000 Uiso D U . . . .
C3 C 0.6200(15) 0.3835(17) 0.7802(9) 0.0099(18) 1.0000 Uiso D U . . . .
C4 C 0.6282(15) 0.510(2) 0.8882(8) 0.0099(18) 1.0000 Uiso D U . . . .
N1 N 0.5275(15) 0.5290(17) 0.6887(8) 0.0102(18) 1.0000 Uiso D U . . . .
N2 N 0.5412(15) 0.7377(17) 0.8661(8) 0.0097(18) 1.0000 Uiso D U . . . .
H11 H 0.3556 1.0726 0.7338 0.0118 1.0000 Uiso R . . . . .
H12 H 0.4416 0.9987 0.6120 0.0118 1.0000 Uiso R . . . . .
H13 H 0.2456 0.8831 0.6444 0.0118 1.0000 Uiso R . . . . .
H31 H 0.6697 0.2222 0.7697 0.0119 1.0000 Uiso R . . . . .
H41 H 0.6847 0.4518 0.9668 0.0119 1.0000 Uiso R . . . . .
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1676(6)
loop_
_oxford_twin_element_scale_factors
1.07(2)
0.08(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
Ag1 . N1 2_666 2.037(8) yes
Ag1 . N1 . 2.037(8) yes
Ag2 . N2 2_677 2.072(8) yes
Ag2 . N2 . 2.072(8) yes
C1 . C2 . 1.479(9) yes
C1 . H11 . 0.950 no
C1 . H12 . 0.950 no
C1 . H13 . 0.950 no
C2 . N1 . 1.339(8) yes
C2 . N2 . 1.338(8) yes
C3 . C4 . 1.352(8) yes
C3 . N1 . 1.368(8) yes
C3 . H31 . 0.950 no
C4 . N2 . 1.381(8) yes
C4 . H41 . 0.950 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
N1 2_666 Ag1 . N1 . 179.994 yes
N2 2_677 Ag2 . N2 . 179.994 yes
C2 . C1 . H11 . 109.5 no
C2 . C1 . H12 . 109.5 no
H11 . C1 . H12 . 109.5 no
C2 . C1 . H13 . 109.5 no
H11 . C1 . H13 . 109.5 no
H12 . C1 . H13 . 109.5 no
C1 . C2 . N1 . 123.1(6) yes
C1 . C2 . N2 . 124.6(6) yes
N1 . C2 . N2 . 112.2(5) yes
C4 . C3 . N1 . 107.8(6) yes
C4 . C3 . H31 . 126.1 no
N1 . C3 . H31 . 126.1 no
C3 . C4 . N2 . 109.1(6) yes
C3 . C4 . H41 . 125.5 no
N2 . C4 . H41 . 125.5 no
C3 . N1 . C2 . 106.1(6) yes
C3 . N1 . Ag1 . 131.9(6) yes
C2 . N1 . Ag1 . 120.9(6) yes
C4 . N2 . C2 . 104.7(6) yes
C4 . N2 . Ag2 . 125.5(6) yes
C2 . N2 . Ag2 . 129.6(6) yes
_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/01/12 at 16:21:14
#
#LIST 12
BLOCK SCALE X'S, U[ISO]
SUMFIX ELEMENT SCALES
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/01/12 at 16:21:14
#
#LIST 16
DIST 1.482,.01= C(1) TO C(2)
DIST 1.345,.01= C(2) TO N(1)
DIST 1.338,.01= C(2) TO N(2)
DIST 1.351,.01= C(3) TO C(4)
DIST 1.371,.01= C(3) TO N(1)
DIST 1.377,.01= C(4) TO N(2)
ANGL 124,1= N(1) TO C(2) TO C(1)
ANGL 124,1= N(2) TO C(2) TO C(1)
ANGL 112,1= N(2) TO C(2) TO N(1)
ANGL 108,1= N(1) TO C(3) TO C(4)
ANGL 109,1= N(2) TO C(4) TO C(3)
ANGL 106,1= C(3) TO N(1) TO C(2)
ANGL 105,1= C(4) TO N(2) TO C(2)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM DELU START (DO NOT REMOVE THIS LINE)
VIBR .0, 0.00200 = C(1) TO C(2)
VIBR .0, 0.00200 = C(2) TO N(1)
VIBR .0, 0.00200 = C(2) TO N(2)
VIBR .0, 0.00500 = N(1) TO C(1)
VIBR .0, 0.00500 = N(2) TO C(1)
VIBR .0, 0.00500 = N(2) TO N(1)
VIBR .0, 0.00200 = C(3) TO C(4)
VIBR .0, 0.00200 = C(3) TO N(1)
VIBR .0, 0.00500 = N(1) TO C(4)
VIBR .0, 0.00200 = C(4) TO N(2)
VIBR .0, 0.00500 = N(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(3)
VIBR .0, 0.00500 = C(2) TO C(4)
REM DELU END (DO NOT REMOVE THIS LINE)
REM THERMSIM START (DO NOT REMOVE THIS LINE)
U(IJ) .0, 0.08000 = C(1) TO C(2)
U(IJ) .0, 0.04000 = C(2) TO N(1)
U(IJ) .0, 0.04000 = C(2) TO N(2)
U(IJ) .0, 0.04000 = C(3) TO C(4)
U(IJ) .0, 0.04000 = C(3) TO N(1)
U(IJ) .0, 0.04000 = C(4) TO N(2)
REM THERMSIM END (DO NOT REMOVE THIS LINE)
PLANAR 0.010000 C(2) C(3) C(4) N(1) N(2)
END
;
#==============================================================================
# start Validation Reply Form
#==============================================================================
_vrf_PLAT022_1.1GPa
;
PROBLEM: Ratio Unique / Expected Reflections (too) Low .. 0.358
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT027_1.1GPa
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 17.38 Deg.
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_1.1GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.378
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_2.2GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.329
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_3.3GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.318
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_3.8GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.321
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_4.9GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.335
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_5.6GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.337
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
_vrf_PLAT029_6.4GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.324
RESPONSE: This is caused by shading of the pressure cell. For more
information please see the experimental special details.
;
#==============================================================================
# end Validation Reply Form
#==============================================================================