# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
_publ_author_address
'Martin M. Kimani'
;Department of Chemistry
Clemson University
Clemson, SC 29634-0973
USA
;
'Julia Brumaghim'
;Department of Chemistry
Clemson University
Clemson, SC 29634-0973
USA
;
_publ_contact_author_address
;Department of Chemistry
Clemson University
Clemson, SC 29634-0973
USA
;
_publ_contact_author_email Brumagh@clemson.edu
_publ_contact_author_phone 864-656-0481
_publ_contact_author_name 'Julia Brumaghim'
# TITLE AND AUTHOR LIST
_publ_section_title
;
ENTER SECTION TITLE
;
data_Cu4(dmise)4I4
_database_code_depnum_ccdc_archive 'CCDC 804911'
_audit_update_record
;
2009-06-04 # Formatted by publCIF
;
_publ_section_title_footnote
;
ENTER FOOTNOTE TO TITLE OF PAPER
;
_publ_section_abstract
;
ENTER ABSTRACT
;
_publ_section_comment
;
ENTER TEXT
;
_publ_section_references
;
ENTER OTHER REFERENCES
Jacobson, R. (1998). REQAB. Version 1.1. Molecular Structure
Corporation, The Woodlands, Texas, USA.
Molecular Structure Corporation & Rigaku (2006). CrystalClear MSC, The
Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). SHELXTL.Version 6.10 Acta Cryst. A64, 112-122.
;
_publ_section_figure_captions
;
ENTER FIGURE CAPTIONS
;
_publ_section_exptl_prep
;
ENTER COMPOUND PREPARATION DETAILS
;
_publ_section_exptl_refinement
;
ENTER SPECIAL DETAILS OF THE REFINEMENT
;
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C21 H33.50 Cu4 I4 N8.50 Se4'
_chemical_formula_sum 'C21 H33.50 Cu4 I4 N8.50 Se4'
_chemical_melting_point ?
_exptl_crystal_description Prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 1482.66
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/m'
_symmetry_int_tables_number 12
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-c 2y'
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'
_cell_length_a 18.802(4)
_cell_length_b 12.883(3)
_cell_length_c 8.4800(17)
_cell_angle_alpha 90.00
_cell_angle_beta 95.07(3)
_cell_angle_gamma 90.00
_cell_volume 2046.0(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 2263
_cell_measurement_theta_min 3.01
_cell_measurement_theta_max 26.71
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.407
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1366
_exptl_absorpt_coefficient_mu 8.652
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.177
_exptl_absorpt_correction_T_max 0.195
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku AFC8S'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 2263
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0366
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 3.01
_diffrn_reflns_theta_max 26.71
_reflns_number_total 2263
_reflns_number_gt 1904
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+7.1423P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2263
_refine_ls_number_parameters 98
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0425
_refine_ls_R_factor_gt 0.0341
_refine_ls_wR_factor_ref 0.0818
_refine_ls_wR_factor_gt 0.0778
_refine_ls_goodness_of_fit_ref 1.107
_refine_ls_restrained_S_all 1.107
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.10117(8) 0.5000 0.0286(2) Uani 1 2 d S . .
Cu2 Cu 0.10112(6) 0.0000 0.28121(16) 0.0402(3) Uani 1 2 d S . .
Se Se 0.03867(3) 0.16416(4) 0.25333(6) 0.01938(14) Uani 1 1 d . . .
I1 I 0.11244(3) 0.0000 0.66602(6) 0.02227(14) Uani 1 2 d S . .
I2 I 0.23169(3) 0.0000 0.20906(6) 0.02688(14) Uani 1 2 d S . .
N1 N 0.1503(2) 0.2993(3) 0.4047(5) 0.0212(9) Uani 1 1 d . . .
N2 N 0.1539(2) 0.2837(4) 0.1521(5) 0.0236(10) Uani 1 1 d . . .
C1 C 0.1186(3) 0.2525(4) 0.2750(6) 0.0201(10) Uani 1 1 d . . .
C2 C 0.1271(4) 0.2964(5) 0.5628(6) 0.0299(13) Uani 1 1 d . . .
H2A H 0.0767 0.3099 0.5580 0.045 Uiso 1 1 calc R . .
H2B H 0.1523 0.3483 0.6270 0.045 Uiso 1 1 calc R . .
H2C H 0.1369 0.2291 0.6083 0.045 Uiso 1 1 calc R . .
C3 C 0.2064(3) 0.3580(4) 0.3637(7) 0.0273(12) Uani 1 1 d . . .
H3A H 0.2373 0.3967 0.4323 0.033 Uiso 1 1 calc R . .
C4 C 0.2088(3) 0.3495(5) 0.2042(7) 0.0310(13) Uani 1 1 d . . .
H4A H 0.2410 0.3816 0.1428 0.037 Uiso 1 1 calc R . .
C5 C 0.1363(4) 0.2536(6) -0.0124(6) 0.0384(16) Uani 1 1 d . . .
H5A H 0.1433 0.1803 -0.0234 0.058 Uiso 1 1 calc R . .
H5B H 0.1667 0.2902 -0.0787 0.058 Uiso 1 1 calc R . .
H5C H 0.0874 0.2706 -0.0435 0.058 Uiso 1 1 calc 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
Cu1 0.0335(6) 0.0258(5) 0.0272(5) 0.000 0.0072(4) 0.000
Cu2 0.0240(6) 0.0193(5) 0.0776(9) 0.000 0.0067(6) 0.000
Se 0.0185(3) 0.0185(3) 0.0209(3) 0.00036(19) 0.0006(2) -0.00177(19)
I1 0.0175(2) 0.0202(2) 0.0286(3) 0.000 -0.00113(19) 0.000
I2 0.0221(3) 0.0311(3) 0.0273(3) 0.000 0.0015(2) 0.000
N1 0.021(2) 0.020(2) 0.023(2) -0.0002(17) 0.0027(18) -0.0053(18)
N2 0.023(2) 0.027(2) 0.020(2) 0.0009(18) 0.0024(18) -0.0069(19)
C1 0.024(3) 0.016(2) 0.020(2) 0.0019(19) 0.002(2) 0.002(2)
C2 0.043(4) 0.028(3) 0.019(3) -0.003(2) 0.006(2) -0.010(3)
C3 0.026(3) 0.025(3) 0.030(3) -0.004(2) -0.003(2) -0.007(2)
C4 0.033(3) 0.031(3) 0.030(3) -0.001(2) 0.008(3) -0.016(3)
C5 0.040(4) 0.056(4) 0.020(3) -0.005(3) 0.007(3) -0.020(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Se 2.4148(8) 2_556 ?
Cu1 Se 2.4148(8) . ?
Cu1 Cu1 2.607(2) 5_556 ?
Cu1 I1 2.7613(9) 5_556 ?
Cu1 I1 2.7613(9) . ?
Cu2 Se 2.4203(9) 6 ?
Cu2 Se 2.4203(9) . ?
Cu2 I2 2.5820(13) . ?
Se C1 1.882(5) . ?
I1 Cu1 2.7613(9) 5_556 ?
N1 C1 1.346(7) . ?
N1 C3 1.367(7) . ?
N1 C2 1.447(6) . ?
N2 C1 1.345(6) . ?
N2 C4 1.378(7) . ?
N2 C5 1.458(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.362(8) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Se Cu1 Se 140.72(5) 2_556 . ?
Se Cu1 Cu1 109.64(3) 2_556 5_556 ?
Se Cu1 Cu1 109.64(3) . 5_556 ?
Se Cu1 I1 108.95(2) 2_556 5_556 ?
Se Cu1 I1 89.57(2) . 5_556 ?
Cu1 Cu1 I1 61.84(2) 5_556 5_556 ?
Se Cu1 I1 89.57(2) 2_556 . ?
Se Cu1 I1 108.95(2) . . ?
Cu1 Cu1 I1 61.84(2) 5_556 . ?
I1 Cu1 I1 123.67(4) 5_556 . ?
Se Cu2 Se 121.81(6) 6 . ?
Se Cu2 I2 116.11(3) 6 . ?
Se Cu2 I2 116.11(3) . . ?
C1 Se Cu1 114.71(15) . . ?
C1 Se Cu2 98.20(16) . . ?
Cu1 Se Cu2 78.60(4) . . ?
Cu1 I1 Cu1 56.33(4) 5_556 . ?
C1 N1 C3 109.6(4) . . ?
C1 N1 C2 126.7(4) . . ?
C3 N1 C2 123.6(5) . . ?
C1 N2 C4 110.0(4) . . ?
C1 N2 C5 125.2(5) . . ?
C4 N2 C5 124.8(5) . . ?
N2 C1 N1 106.7(4) . . ?
N2 C1 Se 123.3(4) . . ?
N1 C1 Se 130.0(4) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 107.6(5) . . ?
C4 C3 H3A 126.2 . . ?
N1 C3 H3A 126.2 . . ?
C3 C4 N2 106.2(5) . . ?
C3 C4 H4A 126.9 . . ?
N2 C4 H4A 126.9 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 26.71
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 1.031
_refine_diff_density_min -0.937
_refine_diff_density_rms 0.174
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.002 165 29 ' '
2 0.000 0.500 -0.007 165 29 ' '
_platon_squeeze_details
;
;
data_Cu(dmise)2I
_database_code_depnum_ccdc_archive 'CCDC 804912'
#TrackingRef '- Kimani Cu halide cif files.pdf'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Cu I N4 Se2'
_chemical_formula_sum 'C10 H16 Cu I N4 Se2'
_chemical_properties_physical 'air-sensitive, moisture-sensitive'
_chemical_melting_point ?
_exptl_crystal_description chip
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 540.63
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_int_tables_number 15
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 15.278(3)
_cell_length_b 10.874(2)
_cell_length_c 11.190(2)
_cell_angle_alpha 90.00
_cell_angle_beta 118.56(3)
_cell_angle_gamma 90.00
_cell_volume 1632.8(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 6421
_cell_measurement_theta_min 2.66
_cell_measurement_theta_max 26.40
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.199
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1016
_exptl_absorpt_coefficient_mu 7.676
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.1994
_exptl_absorpt_correction_T_max 0.2830
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku AFC8S'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 6421
_diffrn_reflns_av_R_equivalents 0.0355
_diffrn_reflns_av_sigmaI/netI 0.0306
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.66
_diffrn_reflns_theta_max 26.40
_reflns_number_total 1674
_reflns_number_gt 1429
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+3.3336P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.00127(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1674
_refine_ls_number_parameters 86
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0395
_refine_ls_R_factor_gt 0.0323
_refine_ls_wR_factor_ref 0.0770
_refine_ls_wR_factor_gt 0.0721
_refine_ls_goodness_of_fit_ref 1.132
_refine_ls_restrained_S_all 1.132
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.0000 0.41055(7) 0.2500 0.0304(2) Uani 1 2 d S . .
I1 I 1.0000 0.17527(3) 0.2500 0.03215(17) Uani 1 2 d S . .
Se1 Se 0.83974(4) 0.48947(4) 0.17239(5) 0.03083(17) Uani 1 1 d . . .
C1 C 0.8545(3) 0.6599(4) 0.1829(4) 0.0255(9) Uani 1 1 d . . .
C2 C 0.9071(4) 0.6867(5) 0.0065(5) 0.0356(11) Uani 1 1 d . . .
H2A H 0.8523 0.6404 -0.0611 0.053 Uiso 1 1 calc R . .
H2B H 0.9650 0.6350 0.0493 0.053 Uiso 1 1 calc R . .
H2C H 0.9210 0.7553 -0.0358 0.053 Uiso 1 1 calc R . .
C3 C 0.8807(4) 0.8532(4) 0.1435(5) 0.0341(11) Uani 1 1 d . . .
H3A H 0.8964 0.9209 0.1066 0.041 Uiso 1 1 calc R . .
C4 C 0.8531(4) 0.8556(4) 0.2400(6) 0.0369(12) Uani 1 1 d . . .
H4A H 0.8460 0.9253 0.2827 0.044 Uiso 1 1 calc R . .
C5 C 0.8059(4) 0.6948(4) 0.3648(6) 0.0372(12) Uani 1 1 d . . .
H5A H 0.8331 0.6148 0.3985 0.056 Uiso 1 1 calc R . .
H5B H 0.7345 0.6910 0.3216 0.056 Uiso 1 1 calc R . .
H5C H 0.8298 0.7520 0.4390 0.056 Uiso 1 1 calc R . .
N1 N 0.8815(3) 0.7313(3) 0.1083(4) 0.0265(8) Uani 1 1 d . . .
N2 N 0.8371(3) 0.7356(3) 0.2651(4) 0.0275(8) Uani 1 1 d . . .
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
Cu1 0.0404(5) 0.0222(4) 0.0318(5) 0.000 0.0199(4) 0.000
I1 0.0386(3) 0.0188(2) 0.0433(3) 0.000 0.0230(2) 0.000
Se1 0.0360(3) 0.0209(2) 0.0391(3) -0.00066(17) 0.0207(2) -0.00364(17)
C1 0.019(2) 0.032(2) 0.024(2) 0.0010(17) 0.0083(18) 0.0002(17)
C2 0.038(3) 0.045(3) 0.030(3) 0.002(2) 0.022(2) -0.008(2)
C3 0.034(3) 0.0167(19) 0.047(3) 0.0039(19) 0.016(2) 0.0009(19)
C4 0.031(3) 0.019(2) 0.056(3) -0.001(2) 0.018(2) 0.0017(19)
C5 0.045(3) 0.036(2) 0.045(3) -0.013(2) 0.033(3) -0.001(2)
N1 0.0251(19) 0.0267(18) 0.026(2) 0.0032(15) 0.0110(16) -0.0038(15)
N2 0.028(2) 0.0248(18) 0.029(2) 0.0017(15) 0.0135(17) 0.0030(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Se1 2.3351(8) 2_755 ?
Cu1 Se1 2.3351(8) . ?
Cu1 I1 2.5585(10) . ?
Se1 C1 1.864(4) . ?
C1 N1 1.341(6) . ?
C1 N2 1.351(6) . ?
C2 N1 1.453(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.334(8) . ?
C3 N1 1.385(6) . ?
C3 H3A 0.9300 . ?
C4 N2 1.381(6) . ?
C4 H4A 0.9300 . ?
C5 N2 1.476(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Se1 Cu1 Se1 136.87(4) 2_755 . ?
Se1 Cu1 I1 111.56(2) 2_755 . ?
Se1 Cu1 I1 111.56(2) . . ?
C1 Se1 Cu1 105.55(13) . . ?
N1 C1 N2 106.9(4) . . ?
N1 C1 Se1 126.9(3) . . ?
N2 C1 Se1 126.2(3) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 107.3(4) . . ?
C4 C3 H3A 126.3 . . ?
N1 C3 H3A 126.3 . . ?
C3 C4 N2 107.5(4) . . ?
C3 C4 H4A 126.2 . . ?
N2 C4 H4A 126.2 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1 N1 C3 109.3(4) . . ?
C1 N1 C2 125.0(4) . . ?
C3 N1 C2 125.8(4) . . ?
C1 N2 C4 109.0(4) . . ?
C1 N2 C5 124.9(4) . . ?
C4 N2 C5 126.2(4) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 26.40
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.197
_refine_diff_density_min -0.793
_refine_diff_density_rms 0.137
data_Cu(dmit)2I(3a)
_database_code_depnum_ccdc_archive 'CCDC 804913'
#TrackingRef '- Kimani Cu halide cif files.pdf'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Cu I N4 S2'
_chemical_formula_sum 'C10 H16 Cu I N4 S2'
_chemical_properties_physical 'air-sensitive, moisture-sensitive'
_exptl_crystal_recrystallization_method
'slow diffusion of ether into acetonitrile'
_chemical_melting_point ?
_exptl_crystal_description Prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 446.83
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_int_tables_number 15
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 15.062(6)
_cell_length_b 10.726(2)
_cell_length_c 11.085(2)
_cell_angle_alpha 90.00
_cell_angle_beta 117.73(2)
_cell_angle_gamma 90.00
_cell_volume 1585.2(8)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 6879
_cell_measurement_theta_min 4.16
_cell_measurement_theta_max 26.76
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.24
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.872
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 872
_exptl_absorpt_coefficient_mu 3.578
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4533
_exptl_absorpt_correction_T_max 0.5463
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_diffrn_measurement_device_type 'Rigaku, AFC8S diffractometer'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 6879
_diffrn_reflns_av_R_equivalents 0.0201
_diffrn_reflns_av_sigmaI/netI 0.0154
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 4.16
_diffrn_reflns_theta_max 26.76
_reflns_number_total 1673
_reflns_number_gt 1624
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.7300P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1673
_refine_ls_number_parameters 85
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0244
_refine_ls_R_factor_gt 0.0237
_refine_ls_wR_factor_ref 0.0583
_refine_ls_wR_factor_gt 0.0577
_refine_ls_goodness_of_fit_ref 1.203
_refine_ls_restrained_S_all 1.203
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I I 0.0000 -0.322234(18) 0.2500 0.02533(9) Uani 1 2 d S . .
Cu Cu 0.0000 -0.08223(4) 0.2500 0.02370(12) Uani 1 2 d S . .
S1 S 0.15384(4) -0.00479(5) 0.31926(6) 0.02525(14) Uani 1 1 d . . .
N1 N 0.16416(13) 0.23230(19) 0.2326(2) 0.0229(4) Uani 1 1 d . . .
N2 N 0.11808(14) 0.22881(19) 0.3902(2) 0.0221(4) Uani 1 1 d . . .
C1 C 0.14427(14) 0.1547(2) 0.3135(2) 0.0191(4) Uani 1 1 d . . .
C5 C 0.0906(2) 0.1833(2) 0.4922(3) 0.0307(5) Uani 1 1 d . . .
H5A H 0.1468 0.1409 0.5631 0.046 Uiso 1 1 calc R . .
H5B H 0.0351 0.1267 0.4502 0.046 Uiso 1 1 calc R . .
H5C H 0.0718 0.2525 0.5304 0.046 Uiso 1 1 calc R . .
C2 C 0.1964(2) 0.1923(3) 0.1334(3) 0.0333(6) Uani 1 1 d . . .
H2A H 0.1670 0.1128 0.0964 0.050 Uiso 1 1 calc R . .
H2B H 0.2682 0.1852 0.1772 0.050 Uiso 1 1 calc R . .
H2C H 0.1753 0.2525 0.0612 0.050 Uiso 1 1 calc R . .
C4 C 0.12140(17) 0.3525(2) 0.3574(3) 0.0298(5) Uani 1 1 d . . .
H4A H 0.1067 0.4213 0.3961 0.036 Uiso 1 1 calc R . .
C3 C 0.14992(17) 0.3546(2) 0.2594(3) 0.0316(5) Uani 1 1 d . . .
H3A H 0.1585 0.4252 0.2172 0.038 Uiso 1 1 calc 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
I 0.03001(14) 0.01446(13) 0.03575(15) 0.000 0.01887(11) 0.000
Cu 0.0315(2) 0.0166(2) 0.0265(2) 0.000 0.01649(17) 0.000
S1 0.0289(3) 0.0156(3) 0.0353(3) 0.0002(2) 0.0183(2) 0.0028(2)
N1 0.0215(9) 0.0217(9) 0.0264(9) 0.0007(8) 0.0120(8) -0.0032(7)
N2 0.0204(8) 0.0212(10) 0.0234(9) -0.0030(8) 0.0090(7) 0.0018(7)
C1 0.0164(9) 0.0193(11) 0.0204(10) -0.0015(8) 0.0076(8) -0.0010(8)
C5 0.0300(12) 0.0416(15) 0.0236(12) -0.0021(10) 0.0151(10) 0.0043(10)
C2 0.0344(13) 0.0412(16) 0.0328(14) 0.0017(10) 0.0229(12) -0.0049(10)
C4 0.0256(10) 0.0173(11) 0.0409(14) -0.0048(10) 0.0109(10) 0.0017(9)
C3 0.0259(11) 0.0171(11) 0.0467(15) 0.0045(11) 0.0128(10) -0.0020(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I Cu 2.5743(6) . ?
Cu S1 2.2345(10) . ?
Cu S1 2.2345(10) 2 ?
S1 C1 1.715(2) . ?
N1 C1 1.355(3) . ?
N1 C3 1.383(3) . ?
N1 C2 1.458(3) . ?
N2 C1 1.350(3) . ?
N2 C4 1.382(3) . ?
N2 C5 1.457(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 C3 1.342(4) . ?
C4 H4A 0.9300 . ?
C3 H3A 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Cu S1 136.36(4) . 2 ?
S1 Cu I 111.823(19) . . ?
S1 Cu I 111.822(19) 2 . ?
C1 S1 Cu 107.59(7) . . ?
C1 N1 C3 109.7(2) . . ?
C1 N1 C2 124.9(2) . . ?
C3 N1 C2 125.5(2) . . ?
C1 N2 C4 110.1(2) . . ?
C1 N2 C5 124.3(2) . . ?
C4 N2 C5 125.6(2) . . ?
N2 C1 N1 105.9(2) . . ?
N2 C1 S1 127.43(17) . . ?
N1 C1 S1 126.65(17) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 N2 107.0(2) . . ?
C3 C4 H4A 126.5 . . ?
N2 C4 H4A 126.5 . . ?
C4 C3 N1 107.3(2) . . ?
C4 C3 H3A 126.3 . . ?
N1 C3 H3A 126.3 . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full 26.76
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max 0.531
_refine_diff_density_min -0.804
_refine_diff_density_rms 0.103
data_Cu(dmit)2I(3b)
_database_code_depnum_ccdc_archive 'CCDC 804914'
#TrackingRef '- Kimani Cu halide cif files.pdf'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Cu I N4 S2'
_chemical_formula_sum 'C10 H16 Cu I N4 S2'
_chemical_properties_physical moisture-sensitive
_exptl_crystal_recrystallization_method
'ether into acetonitrile and dichloromethane'
_chemical_melting_point ?
_exptl_crystal_description Prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 446.83
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_int_tables_number 14
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.925(2)
_cell_length_b 10.861(2)
_cell_length_c 14.868(3)
_cell_angle_alpha 90.00
_cell_angle_beta 92.02(3)
_cell_angle_gamma 90.00
_cell_volume 1601.8(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 13385
_cell_measurement_theta_min 2.05
_cell_measurement_theta_max 26.34
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.853
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 872
_exptl_absorpt_coefficient_mu 3.540
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3622
_exptl_absorpt_correction_T_max 0.5097
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku, AFC8S diffractometer'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 13385
_diffrn_reflns_av_R_equivalents 0.0694
_diffrn_reflns_av_sigmaI/netI 0.0437
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.05
_diffrn_reflns_theta_max 26.34
_reflns_number_total 3225
_reflns_number_gt 3001
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+2.7706P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3225
_refine_ls_number_parameters 167
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0422
_refine_ls_R_factor_gt 0.0386
_refine_ls_wR_factor_ref 0.0943
_refine_ls_wR_factor_gt 0.0916
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.32155(3) 0.89451(2) 0.149492(16) 0.03197(11) Uani 1 1 d . . .
Cu1 Cu 0.16412(4) 0.85343(5) 0.27690(3) 0.02852(14) Uani 1 1 d . . .
S1 S -0.05452(8) 0.80567(10) 0.25502(6) 0.0293(2) Uani 1 1 d . . .
S2 S 0.25345(10) 0.86499(12) 0.41686(6) 0.0364(2) Uani 1 1 d . . .
N1 N -0.1247(3) 0.8960(3) 0.0870(2) 0.0300(7) Uani 1 1 d . . .
N2 N -0.0210(3) 0.7207(3) 0.08446(18) 0.0230(6) Uani 1 1 d . . .
N3 N 0.5207(3) 0.8492(3) 0.3798(2) 0.0322(7) Uani 1 1 d . . .
N4 N 0.4480(3) 1.0366(3) 0.3815(2) 0.0290(6) Uani 1 1 d . . .
C1 C -0.0667(3) 0.8084(3) 0.1399(2) 0.0233(7) Uani 1 1 d . . .
C2 C -0.1875(5) 1.0091(4) 0.1196(3) 0.0474(11) Uani 1 1 d . . .
H2A H -0.2621 0.9882 0.1560 0.071 Uiso 1 1 calc R . .
H2B H -0.2191 1.0576 0.0692 0.071 Uiso 1 1 calc R . .
H2C H -0.1224 1.0554 0.1549 0.071 Uiso 1 1 calc R . .
C3 C -0.1143(4) 0.8631(4) -0.0022(3) 0.0343(8) Uani 1 1 d . . .
H3A H -0.1462 0.9080 -0.0518 0.041 Uiso 1 1 calc R . .
C4 C -0.0498(4) 0.7547(4) -0.0044(2) 0.0311(8) Uani 1 1 d . . .
H4A H -0.0284 0.7106 -0.0556 0.037 Uiso 1 1 calc R . .
C5 C 0.0469(4) 0.6087(4) 0.1142(3) 0.0308(8) Uani 1 1 d . . .
H5A H 0.1162 0.6287 0.1585 0.046 Uiso 1 1 calc R . .
H5B H 0.0865 0.5693 0.0637 0.046 Uiso 1 1 calc R . .
H5C H -0.0172 0.5541 0.1401 0.046 Uiso 1 1 calc R . .
C6 C 0.4102(3) 0.9186(4) 0.3922(2) 0.0265(7) Uani 1 1 d . . .
C7 C 0.5234(6) 0.7152(5) 0.3816(4) 0.0549(13) Uani 1 1 d . . .
H7A H 0.4883 0.6865 0.4372 0.082 Uiso 1 1 calc R . .
H7B H 0.6145 0.6871 0.3767 0.082 Uiso 1 1 calc R . .
H7C H 0.4691 0.6836 0.3321 0.082 Uiso 1 1 calc R . .
C8 C 0.6279(4) 0.9249(4) 0.3602(3) 0.0372(9) Uani 1 1 d . . .
H8A H 0.7151 0.8996 0.3486 0.045 Uiso 1 1 calc R . .
C9 C 0.5833(3) 1.0407(4) 0.3611(3) 0.0334(8) Uani 1 1 d . . .
H9A H 0.6335 1.1111 0.3501 0.040 Uiso 1 1 calc R . .
C10 C 0.3578(4) 1.1421(4) 0.3816(3) 0.0434(10) Uani 1 1 d . . .
H10A H 0.3103 1.1433 0.4367 0.065 Uiso 1 1 calc R . .
H10B H 0.2944 1.1361 0.3316 0.065 Uiso 1 1 calc R . .
H10C H 0.4093 1.2164 0.3766 0.065 Uiso 1 1 calc 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
I1 0.03864(17) 0.02893(18) 0.02845(16) 0.00339(8) 0.00276(11) 0.00018(9)
Cu1 0.0258(2) 0.0313(3) 0.0281(2) -0.00286(17) -0.00399(17) -0.00145(18)
S1 0.0229(4) 0.0442(5) 0.0207(4) -0.0053(4) -0.0001(3) 0.0002(4)
S2 0.0276(4) 0.0574(7) 0.0241(4) 0.0017(4) -0.0006(3) -0.0127(4)
N1 0.0316(16) 0.0271(17) 0.0312(16) -0.0003(12) -0.0002(13) 0.0044(12)
N2 0.0207(12) 0.0268(15) 0.0215(13) 0.0008(11) 0.0000(10) -0.0013(11)
N3 0.0271(15) 0.0288(17) 0.0401(18) -0.0044(14) -0.0061(13) 0.0038(13)
N4 0.0195(13) 0.0346(17) 0.0326(15) -0.0031(13) -0.0016(11) 0.0013(13)
C1 0.0184(14) 0.0289(18) 0.0226(15) -0.0006(13) 0.0002(11) -0.0020(13)
C2 0.058(3) 0.033(2) 0.051(2) 0.001(2) 0.005(2) 0.019(2)
C3 0.0341(19) 0.043(2) 0.0255(17) 0.0078(16) -0.0037(15) 0.0051(17)
C4 0.0308(17) 0.041(2) 0.0213(16) 0.0015(15) 0.0001(13) -0.0014(16)
C5 0.0311(18) 0.031(2) 0.0302(18) 0.0012(14) 0.0033(15) 0.0050(15)
C6 0.0238(16) 0.0338(19) 0.0215(15) -0.0025(14) -0.0036(12) -0.0024(14)
C7 0.055(3) 0.030(2) 0.079(4) -0.005(2) -0.010(3) 0.005(2)
C8 0.0194(17) 0.043(2) 0.050(2) -0.0056(19) 0.0000(15) 0.0028(17)
C9 0.0191(15) 0.036(2) 0.045(2) -0.0036(17) 0.0022(14) -0.0050(15)
C10 0.034(2) 0.039(2) 0.058(3) -0.003(2) 0.0019(19) 0.0075(19)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cu1 2.5373(9) . ?
Cu1 S2 2.2365(12) . ?
Cu1 S1 2.2437(10) . ?
S1 C1 1.712(3) . ?
S2 C6 1.713(4) . ?
N1 C1 1.349(5) . ?
N1 C3 1.381(5) . ?
N1 C2 1.468(5) . ?
N2 C1 1.349(5) . ?
N2 C4 1.391(4) . ?
N2 C5 1.452(5) . ?
N3 C6 1.349(5) . ?
N3 C8 1.384(5) . ?
N3 C7 1.456(6) . ?
N4 C6 1.346(5) . ?
N4 C9 1.388(4) . ?
N4 C10 1.454(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.342(6) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.334(6) . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Cu1 S1 119.84(5) . . ?
S2 Cu1 I1 116.77(3) . . ?
S1 Cu1 I1 123.40(3) . . ?
C1 S1 Cu1 100.05(12) . . ?
C6 S2 Cu1 98.80(12) . . ?
C1 N1 C3 109.4(3) . . ?
C1 N1 C2 125.1(3) . . ?
C3 N1 C2 125.5(4) . . ?
C1 N2 C4 109.3(3) . . ?
C1 N2 C5 124.6(3) . . ?
C4 N2 C5 126.1(3) . . ?
C6 N3 C8 109.4(3) . . ?
C6 N3 C7 124.8(4) . . ?
C8 N3 C7 125.7(4) . . ?
C6 N4 C9 109.4(3) . . ?
C6 N4 C10 125.2(3) . . ?
C9 N4 C10 125.1(4) . . ?
N1 C1 N2 106.7(3) . . ?
N1 C1 S1 127.5(3) . . ?
N2 C1 S1 125.8(3) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 107.6(3) . . ?
C4 C3 H3A 126.2 . . ?
N1 C3 H3A 126.2 . . ?
C3 C4 N2 107.0(3) . . ?
C3 C4 H4A 126.5 . . ?
N2 C4 H4A 126.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 N3 106.5(3) . . ?
N4 C6 S2 127.4(3) . . ?
N3 C6 S2 126.1(3) . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N3 107.5(3) . . ?
C9 C8 H8A 126.3 . . ?
N3 C8 H8A 126.3 . . ?
C8 C9 N4 107.2(4) . . ?
C8 C9 H9A 126.4 . . ?
N4 C9 H9A 126.4 . . ?
N4 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full 26.34
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max 1.119
_refine_diff_density_min -0.988
_refine_diff_density_rms 0.135
data_Cu(dmit)2Cl
_database_code_depnum_ccdc_archive 'CCDC 804915'
#TrackingRef '- Kimani Cu halide cif files.pdf'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Cl Cu N4 S2'
_chemical_formula_sum 'C10 H16 Cl Cu N4 S2'
_chemical_properties_physical 'air-sensitive, moisture-sensitive'
_exptl_crystal_recrystallization_method 'ether into methanol and DMF'
_chemical_melting_point ?
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 355.38
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_int_tables_number 15
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 10.348(2)
_cell_length_b 9.3275(19)
_cell_length_c 16.123(3)
_cell_angle_alpha 90.00
_cell_angle_beta 105.64(3)
_cell_angle_gamma 90.00
_cell_volume 1498.6(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 6865
_cell_measurement_theta_min 2.62
_cell_measurement_theta_max 26.34
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.575
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 728
_exptl_absorpt_coefficient_mu 1.902
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5476
_exptl_absorpt_correction_T_max 0.6797
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe ?
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku, AFC8S diffractometer'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 6856
_diffrn_reflns_av_R_equivalents 0.0231
_diffrn_reflns_av_sigmaI/netI 0.0157
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.62
_diffrn_reflns_theta_max 26.34
_reflns_number_total 1522
_reflns_number_gt 1438
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.9099P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1522
_refine_ls_number_parameters 85
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0318
_refine_ls_R_factor_gt 0.0303
_refine_ls_wR_factor_ref 0.0764
_refine_ls_wR_factor_gt 0.0753
_refine_ls_goodness_of_fit_ref 1.123
_refine_ls_restrained_S_all 1.123
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.21560(4) 0.7500 0.02980(14) Uani 1 2 d S . .
Cl1 Cl 0.5000 -0.02559(8) 0.7500 0.0344(2) Uani 1 2 d S . .
S1 S 0.53525(6) 0.33804(6) 0.63877(3) 0.03211(16) Uani 1 1 d . . .
N1 N 0.55214(18) 0.19132(18) 0.49509(11) 0.0257(4) Uani 1 1 d . . .
C3 C 0.6342(2) 0.0923(2) 0.46965(14) 0.0306(5) Uani 1 1 d . . .
H3A H 0.6236 0.0569 0.4143 0.037 Uiso 1 1 calc R . .
C1 C 0.5995(2) 0.2173(2) 0.58026(13) 0.0238(4) Uani 1 1 d . . .
N2 N 0.70990(17) 0.13503(19) 0.60856(11) 0.0255(4) Uani 1 1 d . . .
C5 C 0.7962(2) 0.1313(3) 0.69647(15) 0.0351(5) Uani 1 1 d . . .
H5A H 0.8243 0.2269 0.7149 0.053 Uiso 1 1 calc R . .
H5B H 0.8735 0.0732 0.6985 0.053 Uiso 1 1 calc R . .
H5C H 0.7475 0.0913 0.7339 0.053 Uiso 1 1 calc R . .
C2 C 0.4348(2) 0.2596(3) 0.43786(15) 0.0356(5) Uani 1 1 d . . .
H2A H 0.3604 0.2532 0.4627 0.053 Uiso 1 1 calc R . .
H2B H 0.4124 0.2121 0.3830 0.053 Uiso 1 1 calc R . .
H2C H 0.4543 0.3586 0.4302 0.053 Uiso 1 1 calc R . .
C4 C 0.7316(2) 0.0576(2) 0.54016(15) 0.0306(5) Uani 1 1 d . . .
H4A H 0.8011 -0.0068 0.5427 0.037 Uiso 1 1 calc 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
Cu1 0.0383(2) 0.0303(2) 0.0233(2) 0.000 0.01275(16) 0.000
Cl1 0.0490(4) 0.0262(4) 0.0265(4) 0.000 0.0074(3) 0.000
S1 0.0505(3) 0.0242(3) 0.0274(3) 0.0054(2) 0.0205(2) 0.0107(2)
N1 0.0294(9) 0.0251(8) 0.0240(9) 0.0042(7) 0.0095(7) -0.0002(7)
C3 0.0407(12) 0.0279(10) 0.0269(11) -0.0047(8) 0.0154(10) -0.0027(9)
C1 0.0288(10) 0.0216(9) 0.0233(10) 0.0038(7) 0.0110(8) -0.0009(7)
N2 0.0292(8) 0.0248(8) 0.0236(8) 0.0015(6) 0.0087(7) 0.0002(7)
C5 0.0339(11) 0.0378(12) 0.0293(11) 0.0019(9) 0.0011(9) 0.0027(9)
C2 0.0400(12) 0.0344(11) 0.0292(11) 0.0079(9) 0.0041(10) 0.0024(10)
C4 0.0316(11) 0.0267(10) 0.0376(12) -0.0033(9) 0.0166(9) 0.0008(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S1 2.2376(6) 2_656 ?
Cu1 S1 2.2376(6) . ?
Cu1 Cl1 2.2497(9) . ?
S1 C1 1.714(2) . ?
N1 C1 1.350(3) . ?
N1 C3 1.389(3) . ?
N1 C2 1.459(3) . ?
C3 C4 1.340(3) . ?
C3 H3A 0.9300 . ?
C1 N2 1.350(3) . ?
N2 C4 1.386(3) . ?
N2 C5 1.458(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 H4A 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Cu1 S1 118.62(3) 2_656 . ?
S1 Cu1 Cl1 120.692(17) 2_656 . ?
S1 Cu1 Cl1 120.692(17) . . ?
C1 S1 Cu1 106.07(7) . . ?
C1 N1 C3 109.67(18) . . ?
C1 N1 C2 125.24(19) . . ?
C3 N1 C2 125.07(19) . . ?
C4 C3 N1 106.85(19) . . ?
C4 C3 H3A 126.6 . . ?
N1 C3 H3A 126.6 . . ?
N2 C1 N1 106.50(17) . . ?
N2 C1 S1 127.31(16) . . ?
N1 C1 S1 126.12(16) . . ?
C1 N2 C4 109.32(18) . . ?
C1 N2 C5 125.67(18) . . ?
C4 N2 C5 124.97(19) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 N2 107.66(19) . . ?
C3 C4 H4A 126.2 . . ?
N2 C4 H4A 126.2 . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 26.34
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 0.700
_refine_diff_density_min -0.397
_refine_diff_density_rms 0.066
data_Cu(dmise)2Cl
_database_code_depnum_ccdc_archive 'CCDC 804916'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Cl Cu N4 Se2'
_chemical_formula_sum 'C10 H16 Cl Cu N4 Se2'
_chemical_properties_physical 'air-sensitive, moisture-sensitive'
_chemical_melting_point ?
_exptl_crystal_description Chip
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15)
_chemical_formula_weight 449.18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_int_tables_number 14
_symmetry_space_group_name_Hall '-P 2ybc'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.794(3)
_cell_length_b 7.0226(14)
_cell_length_c 14.263(3)
_cell_angle_alpha 90.00
_cell_angle_beta 104.64(3)
_cell_angle_gamma 90.00
_cell_volume 1530.7(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15)
_cell_measurement_reflns_used 10854
_cell_measurement_theta_min 2.67
_cell_measurement_theta_max 25.05
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.22
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.949
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 872
_exptl_absorpt_coefficient_mu 6.345
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3476
_exptl_absorpt_correction_T_max 0.4797
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku, AFC8S diffractometer'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 10854
_diffrn_reflns_av_R_equivalents 0.0863
_diffrn_reflns_av_sigmaI/netI 0.0619
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.67
_diffrn_reflns_theta_max 25.05
_reflns_number_total 2713
_reflns_number_gt 2272
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+11.5930P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2713
_refine_ls_number_parameters 167
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0797
_refine_ls_R_factor_gt 0.0684
_refine_ls_wR_factor_ref 0.1868
_refine_ls_wR_factor_gt 0.1680
_refine_ls_goodness_of_fit_ref 1.138
_refine_ls_restrained_S_all 1.138
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Se1 Se 0.86216(5) 0.21544(13) 0.78363(6) 0.0390(3) Uani 1 1 d . . .
Se2 Se 0.63267(5) 0.40018(12) 0.63407(6) 0.0367(3) Uani 1 1 d . . .
Cu1 Cu 0.74637(6) 0.42788(15) 0.77602(7) 0.0345(3) Uani 1 1 d . . .
Cl1 Cl 0.73414(12) 0.6313(3) 0.89265(14) 0.0353(5) Uani 1 1 d . . .
C3 C 0.5213(6) 0.9241(13) 0.6211(6) 0.0365(18) Uani 1 1 d . . .
H3A H 0.5216 1.0561 0.6160 0.044 Uiso 1 1 calc R . .
C1 C 0.5656(5) 0.6193(12) 0.6323(6) 0.0321(16) Uani 1 1 d . . .
N1 N 0.5927(4) 0.8035(9) 0.6289(5) 0.0324(14) Uani 1 1 d . . .
C4 C 0.4527(6) 0.8154(13) 0.6224(6) 0.0379(18) Uani 1 1 d . . .
H4A H 0.3962 0.8581 0.6186 0.045 Uiso 1 1 calc R . .
N2 N 0.4802(4) 0.6257(10) 0.6304(5) 0.0327(14) Uani 1 1 d . . .
C2 C 0.6815(6) 0.8610(13) 0.6321(7) 0.041(2) Uani 1 1 d . . .
H2A H 0.7119 0.7570 0.6115 0.062 Uiso 1 1 calc R . .
H2B H 0.7111 0.8962 0.6972 0.062 Uiso 1 1 calc R . .
H2C H 0.6804 0.9678 0.5898 0.062 Uiso 1 1 calc R . .
C5 C 0.4233(6) 0.4671(14) 0.6318(6) 0.043(2) Uani 1 1 d . . .
H5A H 0.4550 0.3695 0.6734 0.065 Uiso 1 1 calc R . .
H5B H 0.4023 0.4178 0.5673 0.065 Uiso 1 1 calc R . .
H5C H 0.3747 0.5081 0.6557 0.065 Uiso 1 1 calc R . .
N3 N 0.9007(4) 0.2032(9) 0.9930(5) 0.0312(14) Uani 1 1 d . . .
N4 N 1.0140(4) 0.2670(9) 0.9406(5) 0.0321(14) Uani 1 1 d . . .
C7 C 0.8115(5) 0.1509(13) 0.9953(7) 0.0389(19) Uani 1 1 d . . .
H7A H 0.7909 0.0497 0.9500 0.058 Uiso 1 1 calc R . .
H7B H 0.7737 0.2594 0.9782 0.058 Uiso 1 1 calc R . .
H7C H 0.8112 0.1092 1.0594 0.058 Uiso 1 1 calc R . .
C6 C 0.9286(5) 0.2298(11) 0.9115(6) 0.0326(17) Uani 1 1 d . . .
C8 C 1.0719(6) 0.3008(13) 0.8771(7) 0.044(2) Uani 1 1 d . . .
H8A H 1.0499 0.4055 0.8347 0.065 Uiso 1 1 calc R . .
H8B H 1.0742 0.1886 0.8394 0.065 Uiso 1 1 calc R . .
H8C H 1.1295 0.3304 0.9156 0.065 Uiso 1 1 calc R . .
C10 C 1.0418(6) 0.2585(12) 1.0423(6) 0.0357(17) Uani 1 1 d . . .
H10A H 1.0983 0.2773 1.0805 0.043 Uiso 1 1 calc R . .
C9 C 0.9721(5) 0.2187(13) 1.0723(6) 0.0370(19) Uani 1 1 d . . .
H9A H 0.9707 0.2033 1.1366 0.044 Uiso 1 1 calc 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
Se1 0.0342(5) 0.0478(6) 0.0335(5) -0.0019(3) 0.0056(4) 0.0110(3)
Se2 0.0361(5) 0.0309(5) 0.0391(5) -0.0028(3) 0.0020(4) 0.0046(3)
Cu1 0.0292(5) 0.0363(6) 0.0368(6) 0.0012(4) 0.0063(4) 0.0026(4)
Cl1 0.0288(9) 0.0364(10) 0.0402(10) -0.0092(8) 0.0080(8) -0.0008(7)
C3 0.039(5) 0.037(4) 0.034(4) 0.005(3) 0.011(3) 0.008(4)
C1 0.026(4) 0.034(4) 0.034(4) -0.001(3) 0.005(3) -0.002(3)
N1 0.033(3) 0.028(3) 0.034(3) 0.004(3) 0.004(3) -0.002(3)
C4 0.037(4) 0.039(5) 0.035(4) -0.001(3) 0.004(3) 0.009(4)
N2 0.030(3) 0.033(4) 0.033(3) 0.001(3) 0.003(3) -0.005(3)
C2 0.038(5) 0.037(5) 0.051(5) 0.001(4) 0.013(4) -0.012(4)
C5 0.033(4) 0.048(5) 0.046(5) 0.000(4) 0.004(4) -0.024(4)
N3 0.025(3) 0.031(3) 0.040(4) 0.005(3) 0.011(3) -0.003(3)
N4 0.034(4) 0.025(3) 0.035(3) -0.002(3) 0.006(3) -0.002(3)
C7 0.029(4) 0.039(4) 0.051(5) -0.011(4) 0.015(4) -0.006(4)
C6 0.034(4) 0.030(4) 0.034(4) -0.004(3) 0.009(3) 0.009(3)
C8 0.040(5) 0.040(5) 0.056(5) 0.011(4) 0.022(4) 0.004(4)
C10 0.032(4) 0.033(4) 0.037(4) 0.001(3) -0.002(3) 0.001(3)
C9 0.035(4) 0.047(5) 0.030(4) 0.009(3) 0.009(3) 0.006(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 C6 1.862(8) . ?
Se1 Cu1 2.3413(13) . ?
Se2 C1 1.865(8) . ?
Se2 Cu1 2.3505(15) . ?
Cu1 Cl1 2.238(2) . ?
C3 C4 1.329(13) . ?
C3 N1 1.392(11) . ?
C3 H3A 0.9300 . ?
C1 N2 1.343(10) . ?
C1 N1 1.367(10) . ?
N1 C2 1.449(10) . ?
C4 N2 1.397(11) . ?
C4 H4A 0.9300 . ?
N2 C5 1.434(10) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N3 C6 1.356(10) . ?
N3 C9 1.384(11) . ?
N3 C7 1.466(10) . ?
N4 C6 1.333(11) . ?
N4 C10 1.407(10) . ?
N4 C8 1.459(10) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C10 C9 1.308(12) . ?
C10 H10A 0.9300 . ?
C9 H9A 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Se1 Cu1 104.5(2) . . ?
C1 Se2 Cu1 104.6(2) . . ?
Cl1 Cu1 Se1 125.84(7) . . ?
Cl1 Cu1 Se2 120.16(7) . . ?
Se1 Cu1 Se2 113.89(5) . . ?
C4 C3 N1 107.2(8) . . ?
C4 C3 H3A 126.4 . . ?
N1 C3 H3A 126.4 . . ?
N2 C1 N1 106.8(7) . . ?
N2 C1 Se2 126.3(6) . . ?
N1 C1 Se2 126.8(6) . . ?
C1 N1 C3 108.9(7) . . ?
C1 N1 C2 124.8(7) . . ?
C3 N1 C2 126.3(7) . . ?
C3 C4 N2 108.1(7) . . ?
C3 C4 H4A 125.9 . . ?
N2 C4 H4A 125.9 . . ?
C1 N2 C4 108.9(7) . . ?
C1 N2 C5 127.1(7) . . ?
C4 N2 C5 123.9(7) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 N3 C9 108.4(6) . . ?
C6 N3 C7 125.2(7) . . ?
C9 N3 C7 126.2(7) . . ?
C6 N4 C10 110.0(7) . . ?
C6 N4 C8 125.6(7) . . ?
C10 N4 C8 124.4(7) . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C6 N3 106.4(7) . . ?
N4 C6 Se1 126.2(6) . . ?
N3 C6 Se1 127.4(6) . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C10 N4 106.0(7) . . ?
C9 C10 H10A 127.0 . . ?
N4 C10 H10A 127.0 . . ?
C10 C9 N3 109.2(7) . . ?
C10 C9 H9A 125.4 . . ?
N3 C9 H9A 125.4 . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 2.050
_refine_diff_density_min -0.949
_refine_diff_density_rms 0.213
#===================================================================================================================
#===================================================================================================================
#===================================================================================================================
#===================================================================================================================
data_Cu4(dmise)4Br4
_database_code_depnum_ccdc_archive 'CCDC 804917'
#===================================================================================================================
#===================================================================================================================
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C21 H33.50 Br4 Cu4 N8.50 Se4'
_chemical_formula_sum 'C21 H33.50 Br4 Cu4 N8.50 Se4'
_chemical_melting_point ?
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 1294.70
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/m'
_symmetry_int_tables_number 12
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-C 2y'
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'
_cell_length_a 18.374(4)
_cell_length_b 12.867(3)
_cell_length_c 8.4581(17)
_cell_angle_alpha 90.00
_cell_angle_beta 96.71(3)
_cell_angle_gamma 90.00
_cell_volume 1985.9(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 2049
_cell_measurement_theta_min 2.42
_cell_measurement_theta_max 26.26
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.23
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.165
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1222
_exptl_absorpt_coefficient_mu 9.828
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.1506
_exptl_absorpt_correction_T_max 0.2108
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku AFC8S'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 2049
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0205
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_theta_min 2.42
_diffrn_reflns_theta_max 26.26
_reflns_number_total 2049
_reflns_number_gt 1814
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+10.5003P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2049
_refine_ls_number_parameters 98
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0423
_refine_ls_R_factor_gt 0.0379
_refine_ls_wR_factor_ref 0.1079
_refine_ls_wR_factor_gt 0.1042
_refine_ls_goodness_of_fit_ref 1.110
_refine_ls_restrained_S_all 1.110
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.10972(4) 0.0000 1.16098(8) 0.02730(19) Uani 1 2 d S . .
Se1 Se 0.03987(3) 0.16217(4) 0.75442(5) 0.02615(17) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.10223(7) 1.0000 0.0369(3) Uani 1 2 d S . .
Cu2 Cu 0.10584(5) 0.0000 0.75482(12) 0.0374(3) Uani 1 2 d S . .
C1 C 0.1211(3) 0.2532(4) 0.7819(6) 0.0260(10) Uani 1 1 d . . .
N2 N 0.1530(2) 0.2999(3) 0.9147(5) 0.0269(8) Uani 1 1 d . . .
N1 N 0.1583(2) 0.2860(3) 0.6627(5) 0.0314(9) Uani 1 1 d . . .
C4 C 0.2112(3) 0.3622(4) 0.8787(6) 0.0321(11) Uani 1 1 d . . .
H4A H 0.2418 0.4018 0.9504 0.039 Uiso 1 1 calc R . .
C3 C 0.2148(3) 0.3542(5) 0.7214(7) 0.0383(12) Uani 1 1 d . . .
H3A H 0.2481 0.3871 0.6632 0.046 Uiso 1 1 calc R . .
C5 C 0.1284(3) 0.2943(4) 1.0727(6) 0.0349(12) Uani 1 1 d . . .
H5A H 0.0780 0.3155 1.0662 0.052 Uiso 1 1 calc R . .
H5B H 0.1579 0.3396 1.1441 0.052 Uiso 1 1 calc R . .
H5C H 0.1331 0.2243 1.1115 0.052 Uiso 1 1 calc R . .
C2 C 0.1407(4) 0.2560(6) 0.4958(6) 0.0477(16) Uani 1 1 d . . .
H2A H 0.1444 0.1818 0.4863 0.072 Uiso 1 1 calc R . .
H2B H 0.1746 0.2887 0.4331 0.072 Uiso 1 1 calc R . .
H2C H 0.0917 0.2776 0.4584 0.072 Uiso 1 1 calc R . .
Br2 Br 0.23298(4) 0.0000 0.70166(9) 0.0325(2) Uani 1 2 d S . .
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
Br1 0.0202(3) 0.0212(3) 0.0397(4) 0.000 0.0003(3) 0.000
Se1 0.0252(3) 0.0251(3) 0.0280(3) -0.00021(17) 0.00241(19) -0.00151(18)
Cu1 0.0422(6) 0.0332(5) 0.0370(5) 0.000 0.0117(4) 0.000
Cu2 0.0314(5) 0.0258(5) 0.0541(6) 0.000 0.0011(4) 0.000
C1 0.027(2) 0.022(2) 0.030(2) 0.0034(18) 0.0049(19) 0.0013(19)
N2 0.027(2) 0.028(2) 0.0270(19) -0.0001(16) 0.0065(16) -0.0030(17)
N1 0.031(2) 0.034(2) 0.029(2) 0.0022(18) 0.0076(17) -0.0047(19)
C4 0.031(3) 0.028(2) 0.037(3) -0.001(2) 0.002(2) -0.005(2)
C3 0.033(3) 0.040(3) 0.043(3) 0.002(2) 0.011(2) -0.011(2)
C5 0.040(3) 0.035(3) 0.030(2) -0.002(2) 0.005(2) -0.008(2)
C2 0.048(4) 0.070(4) 0.026(3) 0.000(3) 0.008(2) -0.023(3)
Br2 0.0242(4) 0.0351(4) 0.0377(4) 0.000 0.0016(3) 0.000
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.6470(10) 5_557 ?
Br1 Cu1 2.6470(10) . ?
Se1 C1 1.890(5) . ?
Se1 Cu1 2.4087(7) . ?
Se1 Cu2 2.4130(8) . ?
Cu1 Se1 2.4087(7) 2_557 ?
Cu1 Cu1 2.631(2) 5_557 ?
Cu1 Br1 2.6470(10) 5_557 ?
Cu2 Se1 2.4130(8) 6 ?
Cu2 Br2 2.4298(13) . ?
C1 N2 1.346(6) . ?
C1 N1 1.350(6) . ?
N2 C4 1.398(7) . ?
N2 C5 1.462(6) . ?
N1 C3 1.406(7) . ?
N1 C2 1.463(7) . ?
C4 C3 1.344(8) . ?
C4 H4A 0.9300 . ?
C3 H3A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cu1 Br1 Cu1 59.59(4) 5_557 . ?
C1 Se1 Cu1 114.06(15) . . ?
C1 Se1 Cu2 98.41(15) . . ?
Cu1 Se1 Cu2 85.71(4) . . ?
Se1 Cu1 Se1 142.65(5) 2_557 . ?
Se1 Cu1 Cu1 108.68(2) 2_557 5_557 ?
Se1 Cu1 Cu1 108.68(2) . 5_557 ?
Se1 Cu1 Br1 108.22(3) 2_557 5_557 ?
Se1 Cu1 Br1 90.32(3) . 5_557 ?
Cu1 Cu1 Br1 60.20(2) 5_557 5_557 ?
Se1 Cu1 Br1 90.32(3) 2_557 . ?
Se1 Cu1 Br1 108.22(3) . . ?
Cu1 Cu1 Br1 60.20(2) 5_557 . ?
Br1 Cu1 Br1 120.41(4) 5_557 . ?
Se1 Cu2 Se1 119.71(5) 6 . ?
Se1 Cu2 Br2 119.56(3) 6 . ?
Se1 Cu2 Br2 119.56(3) . . ?
N2 C1 N1 105.9(4) . . ?
N2 C1 Se1 129.8(4) . . ?
N1 C1 Se1 124.3(4) . . ?
C1 N2 C4 110.1(4) . . ?
C1 N2 C5 126.2(4) . . ?
C4 N2 C5 123.6(4) . . ?
C1 N1 C3 110.4(4) . . ?
C1 N1 C2 124.4(4) . . ?
C3 N1 C2 125.2(4) . . ?
C3 C4 N2 107.4(5) . . ?
C3 C4 H4A 126.3 . . ?
N2 C4 H4A 126.3 . . ?
C4 C3 N1 106.1(5) . . ?
C4 C3 H3A 127.0 . . ?
N1 C3 H3A 127.0 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full 26.26
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max 1.693
_refine_diff_density_min -1.152
_refine_diff_density_rms 0.153
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 -0.006 159 26 ' '
2 0.000 0.500 -0.016 159 26 ' '
_platon_squeeze_details
;
;
data_Cu(dmit)2Br
_database_code_depnum_ccdc_archive 'CCDC 804918'
#TrackingRef '- Kimani Cu halide cif files.pdf'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Br Cu N4 S2'
_chemical_formula_sum 'C10 H16 Br Cu N4 S2'
_chemical_properties_physical 'air-sensitive, moisture-sensitive'
_exptl_crystal_recrystallization_method 'diethyl ether into acetonitrile'
_chemical_melting_point ?
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 168.15
_chemical_formula_weight 399.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_int_tables_number 15
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 10.385(2)
_cell_length_b 9.5830(19)
_cell_length_c 16.002(3)
_cell_angle_alpha 90.00
_cell_angle_beta 104.15(3)
_cell_angle_gamma 90.00
_cell_volume 1544.2(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 168.15
_cell_measurement_reflns_used 6419
_cell_measurement_theta_min 2.93
_cell_measurement_theta_max 26.27
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.720
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 800
_exptl_absorpt_coefficient_mu 4.261
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3925
_exptl_absorpt_correction_T_max 0.4829
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_measurement_device_type 'Rigaku AFC8S'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 6419
_diffrn_reflns_av_R_equivalents 0.0342
_diffrn_reflns_av_sigmaI/netI 0.0225
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.93
_diffrn_reflns_theta_max 26.27
_reflns_number_total 1552
_reflns_number_gt 1374
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+1.4968P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1552
_refine_ls_number_parameters 86
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0404
_refine_ls_R_factor_gt 0.0346
_refine_ls_wR_factor_ref 0.0884
_refine_ls_wR_factor_gt 0.0842
_refine_ls_goodness_of_fit_ref 1.150
_refine_ls_restrained_S_all 1.150
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.0000 -0.00299(4) 0.7500 0.03625(18) Uani 1 2 d S . .
Cu1 Cu 0.0000 0.24596(6) 0.7500 0.03253(19) Uani 1 2 d S . .
S1 S 0.04874(9) 0.35820(8) 0.63958(5) 0.0353(2) Uani 1 1 d . . .
C1 C 0.1078(3) 0.2296(3) 0.58415(19) 0.0278(6) Uani 1 1 d . . .
N1 N 0.2158(3) 0.1484(3) 0.61299(17) 0.0305(6) Uani 1 1 d . . .
N2 N 0.0577(3) 0.1939(3) 0.50093(16) 0.0303(6) Uani 1 1 d . . .
C4 C 0.1350(3) 0.0907(4) 0.4776(2) 0.0359(7) Uani 1 1 d . . .
H4A H 0.1214 0.0484 0.4239 0.043 Uiso 1 1 calc R . .
C3 C 0.2333(3) 0.0630(3) 0.5472(2) 0.0349(7) Uani 1 1 d . . .
H3A H 0.3009 -0.0019 0.5506 0.042 Uiso 1 1 calc R . .
C5 C -0.0595(4) 0.2561(4) 0.4441(2) 0.0407(8) Uani 1 1 d . . .
H5A H -0.0436 0.3534 0.4365 0.061 Uiso 1 1 calc R . .
H5B H -0.1340 0.2459 0.4692 0.061 Uiso 1 1 calc R . .
H5C H -0.0781 0.2100 0.3892 0.061 Uiso 1 1 calc R . .
C2 C 0.3027(3) 0.1520(4) 0.6995(2) 0.0391(8) Uani 1 1 d . . .
H2A H 0.3284 0.2466 0.7147 0.059 Uiso 1 1 calc R . .
H2B H 0.3805 0.0969 0.7010 0.059 Uiso 1 1 calc R . .
H2C H 0.2566 0.1147 0.7397 0.059 Uiso 1 1 calc 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
Br1 0.0473(3) 0.0273(3) 0.0339(3) 0.000 0.0094(2) 0.000
Cu1 0.0413(3) 0.0318(3) 0.0270(3) 0.000 0.0130(2) 0.000
S1 0.0541(5) 0.0262(4) 0.0313(4) 0.0053(3) 0.0213(4) 0.0084(3)
C1 0.0325(15) 0.0253(15) 0.0277(15) 0.0048(11) 0.0115(12) -0.0029(11)
N1 0.0306(13) 0.0303(13) 0.0316(13) 0.0027(10) 0.0096(11) -0.0021(10)
N2 0.0348(14) 0.0280(14) 0.0302(13) 0.0042(10) 0.0123(10) -0.0009(10)
C4 0.0436(18) 0.0329(17) 0.0350(16) -0.0028(13) 0.0172(14) -0.0024(14)
C3 0.0355(17) 0.0292(16) 0.0442(18) -0.0022(14) 0.0181(14) -0.0008(13)
C5 0.0467(19) 0.0371(19) 0.0362(18) 0.0086(14) 0.0057(15) 0.0008(14)
C2 0.0360(17) 0.0412(19) 0.0366(17) 0.0027(14) 0.0023(14) 0.0007(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.3857(8) . ?
Cu1 S1 2.2298(9) 2_556 ?
Cu1 S1 2.2298(9) . ?
S1 C1 1.717(3) . ?
C1 N2 1.350(4) . ?
C1 N1 1.351(4) . ?
N1 C3 1.380(4) . ?
N1 C2 1.456(4) . ?
N2 C4 1.382(4) . ?
N2 C5 1.456(4) . ?
C4 C3 1.340(5) . ?
C4 H4A 0.9300 . ?
C3 H3A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Cu1 S1 122.32(5) 2_556 . ?
S1 Cu1 Br1 118.84(2) 2_556 . ?
S1 Cu1 Br1 118.84(2) . . ?
C1 S1 Cu1 104.00(10) . . ?
N2 C1 N1 106.2(3) . . ?
N2 C1 S1 126.2(2) . . ?
N1 C1 S1 127.5(2) . . ?
C1 N1 C3 109.5(3) . . ?
C1 N1 C2 125.6(3) . . ?
C3 N1 C2 124.9(3) . . ?
C1 N2 C4 109.8(3) . . ?
C1 N2 C5 125.0(3) . . ?
C4 N2 C5 125.2(3) . . ?
C3 C4 N2 107.0(3) . . ?
C3 C4 H4A 126.5 . . ?
N2 C4 H4A 126.5 . . ?
C4 C3 N1 107.5(3) . . ?
C4 C3 H3A 126.2 . . ?
N1 C3 H3A 126.2 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 26.27
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.155
_refine_diff_density_min -0.489
_refine_diff_density_rms 0.101
data_Cu(dmise)2Br
_database_code_depnum_ccdc_archive 'CCDC 804919'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C10 H16 Br Cu N4 Se2'
_chemical_formula_sum 'C10 H16 Br Cu N4 Se2'
_chemical_properties_physical ' moisture-sensitive'
_exptl_crystal_recrystallization_method
'ether into acetonitrile/dimethylformamide solution'
_chemical_melting_point ?
_exptl_crystal_description prism
_exptl_crystal_colour colorless
_diffrn_ambient_temperature 173.15(2)
_chemical_formula_weight 493.64
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_int_tables_number 15
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 10.297(2)
_cell_length_b 10.390(2)
_cell_length_c 14.824(3)
_cell_angle_alpha 90.00
_cell_angle_beta 101.47(3)
_cell_angle_gamma 90.00
_cell_volume 1554.2(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 173.15(2)
_cell_measurement_reflns_used 6449
_cell_measurement_theta_min 2.80
_cell_measurement_theta_max 26.28
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.110
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 944
_exptl_absorpt_coefficient_mu 8.648
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.1684
_exptl_absorpt_correction_T_max 0.2766
_exptl_absorpt_process_details 'REQAB, CrystalClear'
_exptl_special_details
;
?
;
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku, AFC8S diffractometer'
_diffrn_measurement_method dtprofit.ref
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 6449
_diffrn_reflns_av_R_equivalents 0.0531
_diffrn_reflns_av_sigmaI/netI 0.0360
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.80
_diffrn_reflns_theta_max 26.28
_reflns_number_total 1560
_reflns_number_gt 1411
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC,2006)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC,2006)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC,2006)'
_computing_structure_solution 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_structure_refinement 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_molecular_graphics 'SHELXTL 6.10 (Sheldrick,2008)'
_computing_publication_material 'SHELXTL 6.10 (Sheldrick,2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+7.7997P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1560
_refine_ls_number_parameters 85
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0437
_refine_ls_R_factor_gt 0.0389
_refine_ls_wR_factor_ref 0.0955
_refine_ls_wR_factor_gt 0.0906
_refine_ls_goodness_of_fit_ref 1.114
_refine_ls_restrained_S_all 1.114
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.0000 0.52268(5) 0.2500 0.02954(19) Uani 1 2 d S . .
Se1 Se 0.04871(5) 0.82442(4) 0.40336(3) 0.03082(17) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.75479(7) 0.2500 0.0265(2) Uani 1 2 d S . .
N2 N -0.0099(4) 1.0931(3) 0.3631(2) 0.0264(7) Uani 1 1 d . . .
N1 N 0.1997(4) 1.0597(4) 0.4152(2) 0.0266(7) Uani 1 1 d . . .
C1 C 0.0796(4) 1.0005(4) 0.3940(3) 0.0231(8) Uani 1 1 d . . .
C3 C 0.0527(5) 1.2108(4) 0.3640(3) 0.0325(10) Uani 1 1 d . . .
H3A H 0.0125 1.2893 0.3458 0.039 Uiso 1 1 calc R . .
C2 C 0.1826(5) 1.1907(4) 0.3961(3) 0.0326(10) Uani 1 1 d . . .
H2A H 0.2490 1.2528 0.4042 0.039 Uiso 1 1 calc R . .
C4 C -0.1530(5) 1.0725(5) 0.3364(3) 0.0350(10) Uani 1 1 d . . .
H4A H -0.1711 1.0135 0.2857 0.053 Uiso 1 1 calc R . .
H4B H -0.1962 1.1530 0.3186 0.053 Uiso 1 1 calc R . .
H4C H -0.1856 1.0374 0.3876 0.053 Uiso 1 1 calc R . .
C5 C 0.3270(5) 0.9975(6) 0.4523(4) 0.0390(11) Uani 1 1 d . . .
H5A H 0.3128 0.9077 0.4621 0.058 Uiso 1 1 calc R . .
H5B H 0.3665 1.0371 0.5097 0.058 Uiso 1 1 calc R . .
H5C H 0.3850 1.0069 0.4094 0.058 Uiso 1 1 calc 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
Br1 0.0368(4) 0.0165(3) 0.0347(3) 0.000 0.0057(3) 0.000
Se1 0.0449(3) 0.0211(3) 0.0244(3) 0.00207(15) 0.0016(2) -0.00430(17)
Cu1 0.0291(4) 0.0206(4) 0.0280(4) 0.000 0.0015(3) 0.000
N2 0.0306(19) 0.0254(18) 0.0223(17) -0.0024(14) 0.0034(14) -0.0010(15)
N1 0.0280(18) 0.0277(18) 0.0239(17) -0.0001(14) 0.0045(14) -0.0017(15)
C1 0.031(2) 0.024(2) 0.0134(17) 0.0000(14) 0.0016(15) -0.0026(17)
C3 0.052(3) 0.020(2) 0.026(2) 0.0033(17) 0.007(2) 0.001(2)
C2 0.047(3) 0.026(2) 0.025(2) -0.0027(17) 0.008(2) -0.0137(19)
C4 0.029(2) 0.045(3) 0.029(2) 0.0032(19) 0.0007(18) 0.007(2)
C5 0.027(2) 0.051(3) 0.038(3) 0.000(2) 0.003(2) -0.001(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.4117(10) . ?
Se1 C1 1.867(4) . ?
Se1 Cu1 2.3430(7) . ?
Cu1 Se1 2.3430(7) 2 ?
N2 C1 1.348(6) . ?
N2 C3 1.381(6) . ?
N2 C4 1.464(6) . ?
N1 C1 1.361(6) . ?
N1 C2 1.394(6) . ?
N1 C5 1.467(6) . ?
C3 C2 1.344(7) . ?
C3 H3A 0.9300 . ?
C2 H2A 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Se1 Cu1 103.74(12) . . ?
Se1 Cu1 Se1 144.03(4) . 2 ?
Se1 Cu1 Br1 107.983(19) . . ?
Se1 Cu1 Br1 107.983(19) 2 . ?
C1 N2 C3 110.0(4) . . ?
C1 N2 C4 124.8(4) . . ?
C3 N2 C4 125.1(4) . . ?
C1 N1 C2 108.8(4) . . ?
C1 N1 C5 126.2(4) . . ?
C2 N1 C5 125.0(4) . . ?
N2 C1 N1 106.5(4) . . ?
N2 C1 Se1 127.6(3) . . ?
N1 C1 Se1 125.9(3) . . ?
C2 C3 N2 107.2(4) . . ?
C2 C3 H3A 126.4 . . ?
N2 C3 H3A 126.4 . . ?
C3 C2 N1 107.5(4) . . ?
C3 C2 H2A 126.3 . . ?
N1 C2 H2A 126.3 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 26.28
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max 0.933
_refine_diff_density_min -0.927
_refine_diff_density_rms 0.155