# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?
loop_
_publ_author_name
_publ_author_address
'Ann Chippindale'
;
Department of Chemistry
University of Reading
Reading
Berkshire RG6 6AD
England
;
'Laura J Head'
;
Department of Chemistry
University of Reading
Reading
Berkshire RG6 6AD
England
;
'Simon J Hibble'
;
Department of Chemistry
University of Reading
Reading
Berkshire RG6 6AD
England
;

_publ_contact_author_name        'Ann Chippindale'
_publ_contact_author_email       ANN.CHIPPINDALE@CHEM.OX.AC.UK

_publ_section_title              
;
Simple linear asymmetrical complexes of silver(I):
NC-Ag-NH3 and Br-Ag-NH3
;
_publ_contact_author_address     
;
School of Chemistry
University of Reading
Whiteknights
Reading
Berks RG6 6AD
;
_publ_contact_author_fax         '0118 378 6331'

_publ_contact_author_phone       '0118 378 8448'

# Attachment 'full_use.cif'

data_CRYSTALS1_cif
_database_code_depnum_ccdc_archive 'CCDC 679750'
_audit_creation_date             08-31-01
_audit_creation_method           CRYSTALS_ver_12-03-99
#==============================================================================

_chemical_name_systematic        # IUPAC name, in full
;
Ag(CN)(NH3) at 150K (form II)
;

_chemical_melting_point          ?

# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'
_refine_ls_matrix_type           full

# choose from 'heavy, direct, difmap, geom'
_atom_sites_solution_primary     direct

# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap

# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
_refine_ls_hydrogen_treatment    refall

#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   3.9034(3)
_cell_angle_alpha                90
_cell_length_b                   15.7268(13)
_cell_angle_beta                 90
_cell_length_c                   5.3245(5)
_cell_angle_gamma                90
_cell_volume                     326.86(5)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c m '
_symmetry_space_group_name_Hall  '-P 2c 2b'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,z
x,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x,-y,z+1/2
x,y,-z+1/2

_chemical_absolute_configuration .

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_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B

_cell_formula_units_Z            4
_chemical_formula_sum            ' C H3 Ag N2 '
_chemical_formula_moiety         ' C H3 Ag N2 '
_chemical_compound_source        
;
see paper
;
_chemical_formula_weight         150.92

_cell_measurement_reflns_used    1750
_cell_measurement_theta_min      5
_cell_measurement_theta_max      31
_cell_measurement_temperature    150

_exptl_crystal_description       ' plate '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_max          0.15

_exptl_crystal_density_diffrn    3.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000             280.000
_exptl_absorpt_coefficient_mu    5.889
# Sheldrick geometric definitions 0.41 0.89

_diffrn_measurement_device_type  
;
Oxford Diffraction Gemini S Ultra
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
CrysAlisPro, (Oxford Diffraction, 2006)
;
_computing_data_reduction        
;
CrysAlisPro, (Oxford Diffraction, 2006)
;
_computing_cell_refinement       
;
CrysAlisPro, (Oxford Diffraction, 2006)
;
_computing_structure_solution    
;
SIR92 (Altomare et al, 1994)
;
_diffrn_measurement_method       \w/2\q
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
ABSPACK; (Oxford Diffraction, 2006)
;
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_T_max  0.89

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150(1)
_diffrn_reflns_number            1761
_reflns_number_total             564
_diffrn_reflns_av_R_equivalents  0.014
# Number of reflections with Friedels Law is 564
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 546

_diffrn_reflns_theta_min         5.382
_diffrn_reflns_theta_max         31.883
_diffrn_measured_fraction_theta_max 0.920

_diffrn_reflns_theta_full        30.449
_diffrn_measured_fraction_theta_full 0.973

_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              7

_refine_diff_density_min         -0.39
_refine_diff_density_max         0.76

_refine_ls_number_reflns         391
_refine_ls_number_parameters     32

#_refine_ls_R_factor_ref 0.0154
_refine_ls_wR_factor_ref         0.0170
_refine_ls_goodness_of_fit_ref   1.0466

#_reflns_number_all 564
_refine_ls_R_factor_all          0.0297
_refine_ls_wR_factor_all         0.0171

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                391
_refine_ls_R_factor_gt           0.0154
_refine_ls_wR_factor_gt          0.0170

_refine_ls_shift/su_max          0.000080
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

16.2 -14.2 13.3
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Hydrogen atoms were located in difference Fourier maps.
#Their positions and U[iso] were refined subject to the restraint
#N-H distance = 0.85(1) .

## -------------------REFERENCES ----------------------##
## Insert your own references - in alphabetic order
_publ_section_references         
;

Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C.,
Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution
of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435

Oxford Diffraction (2006). ABSPACK and Crystalis Pro (Version 171.29.8)
Oxford Diffraction Ltd, Abingdon, Oxford, England

Watkin D.J. (1994),
Acta Cryst, A50, 411-437
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.

Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper
R.I. (2001) CRYSTALS
Issue 11. Chemical Crystallography Laboratory, OXFORD, UK.

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 trailing . with the number of unfound
# hydrogen atoms attaced to relavent atom

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_attached_hydrogens
Ag1 Ag 0.24357(5) 0.027604(9) 0.2500 0.0251 1.0000 Uani .
C1 C 0.1621(7) -0.1016(2) 0.2500 0.0215 1.0000 Uani .
N1 N 0.1293(6) -0.17376(14) 0.2500 0.0244 1.0000 Uani .
N2 N 0.3525(6) 0.15989(15) 0.2500 0.0220 1.0000 Uani .
H1 H 0.469(5) 0.1763(18) 0.124(3) 0.050(7) 1.0000 Uiso .
H2 H 0.170(8) 0.189(3) 0.2500 0.063(12) 1.0000 Uiso .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.03185(12) 0.01831(12) 0.02528(12) 0.0000 0.0000 -0.00051(11)
C1 0.0207(8) 0.0247(11) 0.019(1) 0.0000 0.0000 0.0017(8)
N1 0.0260(8) 0.023(1) 0.0238(9) 0.0000 0.0000 -0.0011(9)
N2 0.0241(8) 0.0199(9) 0.0219(9) 0.0000 0.0000 0.0008(8)
_refine_ls_extinction_method     None
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 . C1 . 2.057(3) yes
Ag1 . N2 . 2.123(2) yes
C1 . N1 . 1.142(4) yes
N2 . H1 . 0.85(1) no
N2 . H2 . 0.85(4) 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
C1 . Ag1 . N2 . 177.35(8) yes
Ag1 . C1 . N1 . 177.5(3) yes
Ag1 . N2 . H1 . 113.9(21) no
H1 . N2 . H1 8_555 104.0(34) no
Ag1 . N2 . H2 . 111.3(37) no
H1 . N2 . H2 . 106.6(27) no
#===END
data_CRYSTALS2_cif
_database_code_depnum_ccdc_archive 'CCDC 679751'
_audit_creation_date             08-31-01
_audit_creation_method           CRYSTALS_ver_12-03-99

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

_chemical_name_systematic        
;
Ag(CN)(NH3) at 230K (form I)
;

_chemical_melting_point          ?

# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'
_refine_ls_matrix_type           full

# choose from 'heavy, direct, difmap, geom'
_atom_sites_solution_primary     direct

# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   difmap

# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
_refine_ls_hydrogen_treatment    refall

#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   3.9543(3)
_cell_angle_alpha                90
_cell_length_b                   15.9183(6)
_cell_angle_beta                 90
_cell_length_c                   5.2689(2)
_cell_angle_gamma                90
_cell_volume                     331.65(3)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'C m c m '
_symmetry_space_group_name_Hall  '-C 2c 2'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,z
x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2
-x,-y,z+1/2
x,y,-z+1/2
-x+1/2,-y+1/2,z+1/2
x+1/2,y+1/2,-z+1/2

_chemical_absolute_configuration .

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_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B
'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_IV_Table_2.2B

_cell_formula_units_Z            4
_chemical_formula_sum            ' C H3 Ag N2 '
_chemical_formula_moiety         ' C H3 Ag N2 '
_chemical_compound_source        
;
?
;
_chemical_formula_weight         150.92

_cell_measurement_reflns_used    2300
_cell_measurement_theta_min      5
_cell_measurement_theta_max      32
_cell_measurement_temperature    230

_exptl_crystal_description       ' plate '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.02
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_max          0.15

_exptl_crystal_density_diffrn    3.022
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             280.000
_exptl_absorpt_coefficient_mu    5.804
# Sheldrick geometric definitions 0.42 0.89

_diffrn_measurement_device_type  
;
Oxford Diffraction Gemini S Ultra
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
CrysAlisPro, (Oxford Diffraction, 2006)
;
_computing_data_reduction        
;
CrysAlisPro
;
_computing_cell_refinement       
;
CrysAlisPro
;
_computing_structure_solution    
;
SIR92 (Altomare et al, 1994)
;
_diffrn_measurement_method       \w/2\q
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
ABSPACK, (Oxford Diffraction, 2006)
;
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_T_max  0.89

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      230(1)
_diffrn_reflns_number            2307
_reflns_number_total             330
_diffrn_reflns_av_R_equivalents  0.017
# Number of reflections with Friedels Law is 330
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 290

_diffrn_reflns_theta_min         5.123
_diffrn_reflns_theta_max         32.085
_diffrn_measured_fraction_theta_max 0.932

_diffrn_reflns_theta_full        26.551
_diffrn_measured_fraction_theta_full 0.986

_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              23
_reflns_limit_l_min              0
_reflns_limit_l_max              7

_refine_diff_density_min         -0.57
_refine_diff_density_max         0.36

_refine_ls_number_reflns         264
_refine_ls_number_parameters     24

#_refine_ls_R_factor_ref 0.0166
_refine_ls_wR_factor_ref         0.0156
_refine_ls_goodness_of_fit_ref   1.1035

#_reflns_number_all 330
_refine_ls_R_factor_all          0.0235
_refine_ls_wR_factor_all         0.0182

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                264
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_gt          0.0156

_refine_ls_shift/su_max          0.000677
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

4.41 -1.88 0.845
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

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

# Hydrogen atoms were located in difference Fourier
#maps. The NH3 molecules have two orientations.
#Hydrogen atom postions and U[Iso] were refined with the restraint
#distance N-H = 0.85(1).

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_attached_hydrogens
Ag1 Ag 1.0000 0.72253(2) 0.7500 0.0419 1.0000 Uani .
C1 C 1.0000 0.8514(3) 0.7500 0.0416 1.0000 Uani .
N1 N 1.0000 0.9228(2) 0.7500 0.0426 1.0000 Uani .
N2 N 1.0000 0.5897(2) 0.7500 0.0389 1.0000 Uani .
H1 H 0.821(15) 0.560(6) 0.7500 0.08(3) 0.5000 Uiso .
H2 H 0.889(14) 0.573(3) 0.880(7) 0.07(2) 0.5000 Uiso .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0543(2) 0.03110(15) 0.04021(18) 0.0000 0.0000 0.0000
C1 0.044(3) 0.046(2) 0.035(2) 0.0000 0.0000 0.0000
N1 0.051(2) 0.0369(18) 0.040(2) 0.0000 0.0000 0.0000
N2 0.049(3) 0.0317(17) 0.037(2) 0.0000 0.0000 0.0000
_refine_ls_extinction_method     None
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 . C1 . 2.051(5) yes
Ag1 . N2 . 2.114(4) yes
C1 . N1 . 1.136(6) yes
N2 . H1 . 0.85(1) no
N2 . H1 5_755 0.85(1) no
N2 . H2 . 0.85(1) no
N2 . H2 5_755 0.85(1) no
N2 . H2 10_756 0.85(1) no
N2 . H2 14_556 0.85(1) no
H1 . H2 . 0.76(5) no
H1 . H2 14_556 0.76(5) 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
Ag1 4_666 Ag1 . C1 . 75.131(11) yes
Ag1 4_667 Ag1 . C1 . 75.131(11) yes
Ag1 4_766 Ag1 . C1 . 75.131(11) yes
Ag1 4_767 Ag1 . C1 . 75.131(11) yes
Ag1 4_666 Ag1 . N2 . 104.869(11) yes
Ag1 4_667 Ag1 . N2 . 104.869(11) yes
Ag1 4_766 Ag1 . N2 . 104.869(11) yes
Ag1 4_767 Ag1 . N2 . 104.869(11) yes
C1 . Ag1 . N2 . 180.000 yes
Ag1 . C1 . N1 . 180.000 yes
Ag1 . N2 . H1 . 123.9(71) no
Ag1 . N2 . H1 5_755 123.9(71) no
H1 . N2 . H1 5_755 112.3(143) no
Ag1 . N2 . H2 . 107.8(39) no
H1 . N2 . H2 . 53.3(39) no
H1 5_755 N2 . H2 . 104.8(40) no
Ag1 . N2 . H2 5_755 107.8(39) no
H1 . N2 . H2 5_755 104.8(40) no
H1 5_755 N2 . H2 5_755 53.3(39) no
H2 . N2 . H2 5_755 61.8(88) no
Ag1 . N2 . H2 10_756 107.8(39) no
H1 . N2 . H2 10_756 104.8(40) no
H1 5_755 N2 . H2 10_756 53.3(39) no
H2 . N2 . H2 10_756 144.3(77) no
H2 5_755 N2 . H2 10_756 106.5(80) no
Ag1 . N2 . H2 14_556 107.8(39) no
H1 . N2 . H2 14_556 53.3(39) no
H1 5_755 N2 . H2 14_556 104.8(40) no
H2 . N2 . H2 14_556 106.5(80) no
H2 5_755 N2 . H2 14_556 144.3(77) no
H2 10_756 N2 . H2 14_556 61.8(88) no
N2 . H1 . H2 . 63.3(22) no
N2 . H1 . H2 14_556 63.3(22) no
H2 . H1 . H2 14_556 126.5(45) no
N2 . H2 . H1 . 63.3(22) no
#===END
data_CRYSTALS3_cif
_database_code_depnum_ccdc_archive 'CCDC 679752'
_audit_creation_date             08-31-01
_audit_creation_method           CRYSTALS_ver_12-03-99

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

_chemical_name_systematic        
;
Ag(Br)(NH3)
;

_chemical_melting_point          ?

# choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse'
_refine_ls_matrix_type           full

# choose from 'heavy, direct, difmap, geom'
_atom_sites_solution_primary     direct

# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens   geom

# choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed'
_refine_ls_hydrogen_treatment    mixed

#****************************************************************************
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al 2001)
;
_computing_molecular_graphics    
;
CAMERON (Watkin et al 1996)
;
#=============================================================

_cell_length_a                   4.1931(3)
_cell_angle_alpha                90
_cell_length_b                   5.8730(3)
_cell_angle_beta                 97.553(5)
_cell_length_c                   6.7570(4)
_cell_angle_gamma                90
_cell_volume                     164.955(18)

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

_chemical_absolute_configuration .

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
'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_IV_Table_2.2B
'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_IV_Table_2.2B
'Br ' -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 International_Tables_Vol_IV_Table_2.2B
'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_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' Ag Br H3 N '
_chemical_formula_moiety         ' Ag Br H3 N'
_chemical_compound_source        
;
?
;
_chemical_formula_weight         204.80

_cell_measurement_reflns_used    1400
_cell_measurement_theta_min      5
_cell_measurement_theta_max      32
_cell_measurement_temperature    100

_exptl_crystal_description       ' plate '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.03
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_max          0.13

_exptl_crystal_density_diffrn    4.123
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             184.000
_exptl_absorpt_coefficient_mu    17.922
# Sheldrick geometric definitions 0.17 0.64

_diffrn_measurement_device_type  
;
Oxford Diffraction Gemini S Ultra
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
CrysAlisPro, (Oxford Diffraction, 2006)
;
_computing_data_reduction        
;
CrysAlisPro
;
_computing_cell_refinement       
;
CrysAlisPro
;
_computing_structure_solution    
;
SIR92 (Altomare et al, 1994)
;
_diffrn_measurement_method       \w/2\q
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
ABSPACK; (Oxford Diffraction, 2006)
;
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_T_max  0.59

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      100(1)
_diffrn_reflns_number            1409
_reflns_number_total             575
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections with Friedels Law is 575
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 577

_diffrn_reflns_theta_min         4.616
_diffrn_reflns_theta_max         32.092
_diffrn_measured_fraction_theta_max 0.910

_diffrn_reflns_theta_full        30.006
_diffrn_measured_fraction_theta_full 0.996

_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_reflns_limit_h_min              -5
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              8
_reflns_limit_l_min              0
_reflns_limit_l_max              9

_refine_diff_density_min         -2.45
_refine_diff_density_max         1.03

_refine_ls_number_reflns         464
_refine_ls_number_parameters     24

#_refine_ls_R_factor_ref 0.0264
_refine_ls_wR_factor_ref         0.0295
_refine_ls_goodness_of_fit_ref   0.8882

#_reflns_number_all 575
_refine_ls_R_factor_all          0.0317
_refine_ls_wR_factor_all         0.0295

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                464
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_gt          0.0295

_refine_ls_shift/su_max          0.009306
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

30.4 -26.9 22.3
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

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

# Hydrogen atoms were located in difference Fourier maps.
#Their positions were refined subject to the restraint
#N-H distance = 0.85(1) and H-N-H angle = 109(5).
#U[iso] were fixed at 0.05A-2.

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_attached_hydrogens
Ag1 Ag 0.66743(9) 0.2500 0.03322(5) 0.0168 1.0000 Uani .
Br1 Br 1.0431(1) 0.2500 -0.23183(7) 0.0116 1.0000 Uani .
N1 N 0.4612(11) 0.2500 0.3150(7) 0.0154 1.0000 Uani .
H1 H 0.605(16) 0.2500 0.416(9) 0.0500 1.0000 Uiso .
H2 H 0.356(13) 0.374(6) 0.314(8) 0.0500 1.0000 Uiso .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag1 0.0175(2) 0.0193(2) 0.0144(2) 0.0000 0.00478(13) 0.0000
Br1 0.0098(2) 0.0126(2) 0.0121(2) 0.0000 0.00043(15) 0.0000
N1 0.0146(18) 0.0148(18) 0.0154(19) 0.0000 -0.0031(14) 0.0000
_refine_ls_extinction_method     None
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 . Ag1 2_655 3.2604(3) yes
Ag1 . Br1 1_455 2.9714(5) yes
Ag1 . Br1 . 2.5358(5) yes
Ag1 . N1 . 2.192(5) yes
N1 . H1 . 0.85(6) no
N1 . H2 . 0.85(4) no
N1 . H2 4_555 0.85(4) 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
Br1 . Ag1 . N1 . 165.01(12) yes
Ag1 . N1 . H1 . 112.4(64) no
Ag1 . N1 . H2 . 105.1(43) no
H1 . N1 . H2 . 108.4(29) no
Ag1 . N1 . H2 4_555 105.1(43) no
H1 . N1 . H2 4_555 108.4(29) no
H2 . N1 . H2 4_555 117.5(88) no