# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2006

data_global

_journal_coden_Cambridge         440

loop_
_publ_author_name
'A. Williams'
'Gerald Bernardinelli'
'Bernard Bocquet'
'Anita Kubel-Pollak'
'Francine Lavergnat'
'Craig J. Matthews'
'Xavier Melich'
'Pierre-Yves Morgantini'
'Simon Verdan'

_publ_contact_author_name        'A. Williams'
_publ_contact_author_address     
;
Dept of Inorganic, Analytical & Applied Chemistry
University of Geneva
30 quai E. Ansernet
Geneva 4
CH-1211
SWITZERLAND
;

_publ_contact_author_email       ALAN.WILLIAMS@CHIAM.UNIGE.CH

_publ_requested_journal          'New Journal of Chemistry'

_publ_section_title              
;
Conformational effects in molecular tectons containing
protonated benzimidazole cations.
;

# Attachment '1bH2.cif'

data_1bH2
_database_code_depnum_ccdc_archive 'CCDC 602150'

#-- (C18H20N4)MnCl4 -------------------------------------- [1bH2][MnCl4] ---

_audit_creation_date             1997-09-04
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2005-12-05
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1

_chemical_formula_moiety         'C18 H20 Cl4 Mn N4'
_chemical_formula_sum            'C18 H20 Cl4 Mn N4'
_chemical_formula_weight         489.1

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C mca'
_symmetry_space_group_name_Hall  '-C 2bc 2'

loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2-y,1/2+z
+x,-y,-z
-x,1/2+y,1/2-z
-x,-y,-z
+x,1/2+y,1/2-z
-x,+y,+z
+x,1/2-y,1/2+z
1/2+x,1/2+y,+z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
1/2-x,+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,+y,1/2-z
1/2-x,1/2+y,+z
1/2+x,-y,1/2+z
_cell_length_a                   16.6400(10)
_cell_length_b                   13.2690(10)
_cell_length_c                   18.7700(10)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_volume                     4144.3(5)
_cell_formula_units_Z            8
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      not_measured
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      22.5
_cell_measurement_theta_max      29.5
_cell_measurement_temperature    200
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    10.015
_exptl_crystal_description       plate
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .07
_exptl_crystal_colour            colorless

_diffrn_measurement_device_type  Stoe_Stadi-4_4-circle_diffractometer
_diffrn_measurement_method       \w-2\q_scans
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'xtal_lsabs (Flack & al. 1992)'
_exptl_absorpt_correction_T_min  .0663
_exptl_absorpt_correction_T_max  .4876
_diffrn_reflns_number            2633
_reflns_number_total             1325
_reflns_number_gt                1148
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_diffrn_reflns_theta_max         54.9
_diffrn_reflns_theta_full        54.9
_diffrn_measured_fraction_theta_max 1.
_diffrn_measured_fraction_theta_full 1.
_diffrn_reflns_av_R_equivalents  .048
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         2
_diffrn_standards_interval_time  45
_diffrn_standards_decay_%        0

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .046
_refine_ls_wR_factor_ref         .044
_refine_ls_goodness_of_fit_ref   1.58(3)
_refine_ls_number_reflns         1148
_refine_ls_number_parameters     158
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.0001(Fo^2^)]
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          .0034
_refine_diff_density_max         .567
_refine_diff_density_min         -.596
_refine_ls_extinction_method     Zachariasen
_refine_ls_extinction_coef       2639(400)

_refine_special_details          
;
Hydrogen treatment:

Observed and refined with a fixed value of the isotropic displacement
parameters.
Hydrogen atoms of the methyl groups have been refined with restraints
on the bond lengths and bond angles.
;

_computing_data_collection       Stoe_Stadi-4
_computing_cell_refinement       xtal_latcon
_computing_data_reduction        xtal_REFCAL_LSABS__SORTRF
_computing_structure_solution    multan_87
_computing_structure_refinement  xtal_CRYLSQ
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO

loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003
Mn Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .295 .729
Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .132 .159

loop_
_atom_site_label
_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
Mn .00000 .19095(8) .68927(5) .03614 1.00000 Uani
Cl1 .00000 .37274(13) .69253(9) .04682 1.00000 Uani
Cl2 .00000 .14430(14) .56805(8) .04579 1.00000 Uani
Cl3 .12264(7) .14029(10) .73869(6) .05229 1.00000 Uani
N1 .3188(3) .1208(4) .37451(18) .03903 1.00000 Uani
N2 .1931(3) .1163(3) .40703(17) .03684 1.00000 Uani
C1 .2434(3) .1156(4) .3513(3) .03297 1.00000 Uani
C2 .3175(3) .1253(4) .4495(3) .03761 1.00000 Uani
C3 .3805(3) .1295(5) .4987(3) .05027 1.00000 Uani
C4 .3572(4) .1322(5) .5698(3) .05011 1.00000 Uani
C5 .2765(4) .1306(4) .5900(3) .04479 1.00000 Uani
C6 .2157(4) .1258(4) .5416(3) .04140 1.00000 Uani
C7 .2383(3) .1216(4) .4697(3) .03767 1.00000 Uani
C8 .1058(3) .1091(5) .4022(3) .04747 1.00000 Uani
C9 .2162(4) .1123(5) .2760(3) .03714 1.00000 Uani
H1 .366(3) .125(4) .346(3) .05000 1.00000 Uiso
H3 .438(3) .147(4) .486(3) .05000 1.00000 Uiso
H4 .398(3) .130(4) .607(3) .05000 1.00000 Uiso
H5 .265(3) .130(4) .644(3) .05000 1.00000 Uiso
H6 .155(3) .124(4) .554(3) .05000 1.00000 Uiso
H81 .0907(13) .0365(16) .3806(14) .05000 1.00000 Uiso
H82 .0796(13) .119(3) .4521(11) .05000 1.00000 Uiso
H83 .0842(14) .1650(18) .3668(13) .05000 1.00000 Uiso
H91 .185(3) .061(4) .271(3) .05000 1.00000 Uiso
H92 .183(3) .163(4) .268(3) .05000 1.00000 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mn .03961 .04424 .02458 .00000 .00000 -.00301
Cl1 .04335 .04248 .05464 .00000 .00000 -.00611
Cl2 .04590 .06605 .02543 .00000 .00000 -.00648
Cl3 .05660 .06006 .04020 .00890 -.01280 -.00103
N1 .04364 .05012 .02333 -.01427 .00280 .00773
N2 .04275 .04491 .02285 -.01441 -.00306 .00050
C1 .03773 .03588 .02531 -.01036 -.00016 .00055
C2 .04525 .04250 .02509 -.01637 .00013 .00329
C3 .03861 .07406 .03815 -.01946 -.00553 .00949
C4 .05678 .06208 .03148 -.01620 -.01100 .00570
C5 .06089 .04702 .02646 -.01914 -.00623 .00002
C6 .04760 .04769 .02890 -.01936 .00073 -.00064
C7 .04724 .04279 .02297 -.02312 -.00496 .00447
C8 .04081 .07356 .02805 -.02030 -.00665 -.00442
C9 .03878 .04952 .02313 -.00817 -.00015 .00185

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn Cl2 . . 2.3580(19)
Mn Cl3 . . 2.3403(13)
Mn Cl3 . 7 2.3403(13)
N1 C1 . . 1.329(7)
N1 C2 . . 1.410(6)
N1 H1 . . .96(5)
N2 C1 . . 1.340(6)
N2 C7 . . 1.398(6)
N2 C8 . . 1.458(6)
C1 C9 . . 1.485(7)
C2 C3 . . 1.398(7)
C2 C7 . . 1.372(7)
C3 C4 . . 1.391(7)
C3 H3 . . 1.01(5)
C4 C5 . . 1.395(8)
C4 H4 . . .97(5)
C5 C6 . . 1.361(7)
C5 H5 . . 1.04(5)
C6 C7 . . 1.402(6)
C6 H6 . . 1.03(5)
C8 H81 . . 1.08(3)
C8 H82 . . 1.04(3)
C8 H83 . . 1.06(3)
C9 H91 . . .86(5)
C9 H92 . . .89(5)
C9 C9 . 12 1.489(8)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
Cl2 Mn Cl3 . . . 107.88(5)
Cl2 Mn Cl3 . . 7 107.88(5)
Cl3 Mn Cl3 . . 7 121.38(6)
C1 N1 C2 . . . 108.4(4)
C1 N1 H1 . . . 126(3)
C2 N1 H1 . . . 125(3)
C1 N2 C7 . . . 108.7(4)
C1 N2 C8 . . . 125.0(4)
C7 N2 C8 . . . 126.2(4)
N1 C1 N2 . . . 109.5(4)
N1 C1 C9 . . . 126.9(4)
N2 C1 C9 . . . 123.6(5)
N1 C2 C3 . . . 130.5(5)
N1 C2 C7 . . . 106.8(4)
C3 C2 C7 . . . 122.7(5)
C2 C3 C4 . . . 115.2(5)
C2 C3 H3 . . . 124(3)
C4 C3 H3 . . . 119(3)
C3 C4 C5 . . . 121.8(5)
C3 C4 H4 . . . 120(3)
C5 C4 H4 . . . 118(3)
C4 C5 C6 . . . 122.4(5)
C4 C5 H5 . . . 117(3)
C6 C5 H5 . . . 121(3)
C5 C6 C7 . . . 116.4(5)
C5 C6 H6 . . . 125(3)
C7 C6 H6 . . . 118(3)
N2 C7 C2 . . . 106.7(4)
N2 C7 C6 . . . 131.9(5)
C2 C7 C6 . . . 121.4(5)
N2 C8 H81 . . . 108.4(13)
N2 C8 H82 . . . 110.7(13)
N2 C8 H83 . . . 109.4(13)
H81 C8 H82 . . . 111(2)
H81 C8 H83 . . . 108.1(19)
H82 C8 H83 . . . 110(2)
C1 C9 H91 . . . 108(3)
C1 C9 H92 . . . 109(3)
C1 C9 C9 . . 12 113.2(5)
H91 C9 H92 . . . 102(5)
H91 C9 C9 . . 12 113(3)
H92 C9 C9 . . 12 112(3)

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
C2 N1 C1 N2 . . . . -.0(6)
C2 N1 C1 C9 . . . . 178.3(5)
H1 N1 C1 N2 . . . . -177(4)
H1 N1 C1 C9 . . . . 2(4)
C1 N1 C2 C3 . . . . 178.6(6)
C1 N1 C2 C7 . . . . .5(6)
H1 N1 C2 C3 . . . . -5(4)
H1 N1 C2 C7 . . . . 177(4)
C7 N2 C1 N1 . . . . -.4(6)
C7 N2 C1 C9 . . . . -178.8(5)
C8 N2 C1 N1 . . . . -178.4(5)
C8 N2 C1 C9 . . . . 3.2(8)
C1 N2 C7 C2 . . . . .7(6)
C1 N2 C7 C6 . . . . 179.0(5)
C8 N2 C7 C2 . . . . 178.7(5)
C8 N2 C7 C6 . . . . -3.0(9)
C1 N2 C8 H81 . . . . 64.4(16)
C1 N2 C8 H82 . . . . -174.1(17)
C1 N2 C8 H83 . . . . -53.2(15)
C7 N2 C8 H81 . . . . -113.3(15)
C7 N2 C8 H82 . . . . 8.2(18)
C7 N2 C8 H83 . . . . 129.1(15)
N1 C1 C9 H91 . . . . 128(4)
N1 C1 C9 H92 . . . . -123(4)
N1 C1 C9 C9 . . . 12 1.8(8)
N2 C1 C9 H91 . . . . -54(4)
N2 C1 C9 H92 . . . . 55(4)
N2 C1 C9 C9 . . . 12 179.9(5)
N1 C2 C3 C4 . . . . -179.4(5)
N1 C2 C3 H3 . . . . 15(4)
C7 C2 C3 C4 . . . . -1.5(8)
C7 C2 C3 H3 . . . . -167(3)
N1 C2 C7 N2 . . . . -.7(6)
N1 C2 C7 C6 . . . . -179.2(5)
C3 C2 C7 N2 . . . . -179.0(5)
C3 C2 C7 C6 . . . . 2.5(8)
C2 C3 C4 C5 . . . . .1(8)
C2 C3 C4 H4 . . . . 175(4)
H3 C3 C4 C5 . . . . 166(3)
H3 C3 C4 H4 . . . . -19(5)
C3 C4 C5 C6 . . . . .3(9)
C3 C4 C5 H5 . . . . 178(3)
H4 C4 C5 C6 . . . . -175(4)
H4 C4 C5 H5 . . . . 3(5)
C4 C5 C6 C7 . . . . .6(8)
C4 C5 C6 H6 . . . . 179(3)
H5 C5 C6 C7 . . . . -177(3)
H5 C5 C6 H6 . . . . 2(5)
C5 C6 C7 N2 . . . . 180.0(5)
C5 C6 C7 C2 . . . . -1.9(8)
H6 C6 C7 N2 . . . . 1(3)
H6 C6 C7 C2 . . . . 179(3)

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 Cl1 . . 11_556 0.96(4) 2.34(5) 2.269(4) 163(4)

#=END======================================================================

# Attachment '3bH2Cl.cif'

data_3bH2Cl
_database_code_depnum_ccdc_archive 'CCDC 602151'

#--((C22H26N4)Cl2)2 (CH3CN)---------------------- [3bH2]Cl2 0.5CH3CN ---

_audit_creation_date             1999-01-05
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2005-12-05
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1

_chemical_formula_moiety         '(C22 H26 N4)2 , 4Cl , (C2 H3 N)'
_chemical_formula_sum            'C46 H55 Cl4 N9'
_chemical_formula_weight         875.8

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a                   15.483(3)
_cell_length_b                   12.7050(10)
_cell_length_c                   23.177(2)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.971(8)
_cell_angle_gamma                90.00000
_cell_volume                     4558.5(10)
_cell_formula_units_Z            4
_exptl_crystal_F_000             1848
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      not_measured
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54183
_cell_measurement_reflns_used    30
_cell_measurement_theta_min      15.5
_cell_measurement_theta_max      19.5
_cell_measurement_temperature    200
_exptl_absorpt_coefficient_mu    2.693
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_colour            colorless

_diffrn_measurement_device_type  Stoe_Stadi-4_4-circle_diffractometer
_diffrn_measurement_method       \w-2\q_scans
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'xtal_lsabs (Flack & al. 1992)'
_exptl_absorpt_correction_T_min  .525229
_exptl_absorpt_correction_T_max  .676566
_diffrn_reflns_number            5679
_reflns_number_total             5515
_reflns_number_gt                3676
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_diffrn_reflns_theta_max         54
_diffrn_reflns_theta_full        54
_diffrn_measured_fraction_theta_max 1.
_diffrn_measured_fraction_theta_full 1.
_diffrn_reflns_av_R_equivalents  .051
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         2
_diffrn_standards_interval_time  45
_diffrn_standards_decay_%        0

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .066
_refine_ls_wR_factor_ref         .062
_refine_ls_goodness_of_fit_ref   1.25(1)
_refine_ls_number_reflns         3676
_refine_ls_number_parameters     533
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     \w=1/[\s^2(Fo)+0.0003(Fo^2)]
_refine_ls_hydrogen_treatment    noref
_refine_ls_shift/su_max          .00024
_refine_diff_density_max         .64
_refine_diff_density_min         -.603
_refine_ls_extinction_method     Zachariasen
_refine_ls_extinction_coef       1860(424)
_refine_ls_abs_structure_details none

_refine_special_details          
;
Hydrogen treatment:

Calculated excepted for:
- H(methyl) refined with restraints on bond lengths and bond angles and
then blocked in the last cycles.
- H(N+) refined without restraint and blocked in the last cycles.
;

_computing_data_collection       Stoe_Stadi-4
_computing_cell_refinement       Xtal_latcon
_computing_data_reduction        xtal_REFCAL_LSABS__SORTRF
_computing_structure_solution    Multan87
_computing_structure_refinement  xtal_CRYLSQ
_computing_molecular_graphics    Xtal_Gx3
_computing_publication_material  xtal_CIFIO

loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .017 .009
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .029 .018
Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .348 .702

loop_
_atom_site_label
_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
Cl1 .05642(11) .69430(14) .69835(8) .0423(11) 1.00000 Uani
Cl2 .07282(11) .63876(15) .42643(8) .0463(12) 1.00000 Uani
Cl3 .35913(11) .15069(14) .55603(8) .0466(12) 1.00000 Uani
Cl4 .59182(14) .83460(18) .63888(10) .0715(16) 1.00000 Uani
N1a .3351(4) .9124(5) .7033(3) .031(4) 1.00000 Uani
N2a .2144(3) .8265(4) .7113(3) .028(4) 1.00000 Uani
N3a .3497(3) .8670(4) .4427(3) .029(4) 1.00000 Uani
N4a .2320(4) .7762(5) .4311(3) .032(4) 1.00000 Uani
C1a .2634(4) .8621(6) .5722(3) .029(4) 1.00000 Uani
C2a .2327(4) .9067(6) .5132(3) .030(4) 1.00000 Uani
C3a .1330(4) .9087(6) .5099(3) .032(4) 1.00000 Uani
C4a .0987(4) .9795(6) .5577(3) .034(5) 1.00000 Uani
C5a .1280(4) .9398(6) .6171(3) .035(5) 1.00000 Uani
C6a .2281(4) .9328(5) .6206(3) .029(4) 1.00000 Uani
C7a .2578(4) .8922(5) .6779(3) .026(4) 1.00000 Uani
C8a .3415(4) .8562(6) .7545(3) .031(5) 1.00000 Uani
C9a .4080(4) .8484(6) .7965(3) .035(5) 1.00000 Uani
C10a .3925(5) .7839(6) .8427(3) .037(5) 1.00000 Uani
C11a .3143(5) .7298(6) .8474(3) .037(5) 1.00000 Uani
C12a .2486(4) .7362(6) .8069(3) .034(5) 1.00000 Uani
C13a .2650(4) .8012(5) .7599(3) .028(4) 1.00000 Uani
C14a .2714(4) .8496(5) .4635(3) .027(4) 1.00000 Uani
C15a .3610(4) .8045(6) .3940(3) .028(4) 1.00000 Uani
C16a .4286(5) .7972(6) .3558(3) .036(5) 1.00000 Uani
C17a .4174(5) .7297(6) .3095(3) .042(5) 1.00000 Uani
C18a .3400(5) .6722(6) .3025(3) .044(5) 1.00000 Uani
C19a .2736(5) .6788(6) .3405(3) .042(5) 1.00000 Uani
C20a .2855(4) .7476(6) .3869(3) .030(5) 1.00000 Uani
C21a .4030(4) .9833(6) .6824(3) .040(5) 1.00000 Uani
C22a .4151(4) .9408(6) .4649(3) .041(5) 1.00000 Uani
N1b .1937(4) .4889(4) .5751(3) .029(4) 1.00000 Uani
N2b .2921(4) .3739(5) .5550(3) .034(4) 1.00000 Uani
N3b .1943(4) .4377(5) .2797(3) .031(4) 1.00000 Uani
N4b .2948(4) .3347(5) .3134(3) .042(4) 1.00000 Uani
C1b .2204(5) .3946(6) .4321(3) .035(5) 1.00000 Uani
C2b .1686(4) .3576(6) .3781(3) .029(4) 1.00000 Uani
C3b .1426(4) .2423(6) .3837(3) .036(5) 1.00000 Uani
C4b .0887(5) .2255(6) .4373(3) .040(5) 1.00000 Uani
C5b .1366(5) .2639(6) .4924(3) .035(5) 1.00000 Uani
C6b .1657(4) .3795(5) .4862(3) .031(4) 1.00000 Uani
C7b .2157(5) .4133(6) .5388(3) .032(5) 1.00000 Uani
C8b .2594(4) .4988(6) .6177(3) .032(5) 1.00000 Uani
C9b .2665(5) .5647(6) .6652(3) .041(5) 1.00000 Uani
C10b .3419(5) .5533(6) .6988(3) .045(5) 1.00000 Uani
C11b .4050(5) .4795(6) .6848(4) .051(6) 1.00000 Uani
C12b .3965(5) .4125(6) .6378(4) .046(5) 1.00000 Uani
C13b .3207(4) .4248(6) .6048(3) .033(5) 1.00000 Uani
C14b .2174(4) .3769(6) .3246(3) .032(5) 1.00000 Uani
C15b .2579(5) .4340(6) .2383(3) .033(5) 1.00000 Uani
C16b .2660(5) .4862(6) .1858(3) .042(5) 1.00000 Uani
C17b .3402(6) .4670(6) .1560(4) .050(6) 1.00000 Uani
C18b .4051(6) .4003(7) .1774(4) .061(6) 1.00000 Uani
C19b .3974(5) .3499(7) .2306(4) .052(6) 1.00000 Uani
C20b .3221(5) .3686(6) .2605(3) .037(5) 1.00000 Uani
C21b .1138(5) .5518(6) .5726(3) .040(5) 1.00000 Uani
C22b .1117(5) .4952(6) .2740(3) .039(5) 1.00000 Uani
C01 .4215(7) .6308(8) .5204(5) .072(7) 1.00000 Uani
C02 .5084(7) .6474(9) .5389(6) .132(11) 1.00000 Uani
N01 .3540(6) .6167(7) .5067(4) .101(7) 1.00000 Uani
H02a .15534 .78707 .70255 .05000 1.00000 Uiso
H04a .17247 .74802 .43756 .05000 1.00000 Uiso
H011a .23940 .78234 .57739 .05000 1.00000 Uiso
H012a .33379 .86199 .57446 .05000 1.00000 Uiso
H2a .25612 .98707 .50943 .05000 1.00000 Uiso
H31a .11179 .93907 .46812 .05000 1.00000 Uiso
H32a .10806 .82908 .51558 .05000 1.00000 Uiso
H41a .12280 1.05931 .55164 .05000 1.00000 Uiso
H42a .02821 .98018 .55551 .05000 1.00000 Uiso
H51a .10542 .99370 .65021 .05000 1.00000 Uiso
H52a .10071 .86183 .62443 .05000 1.00000 Uiso
H6a .25298 1.01235 .61524 .05000 1.00000 Uiso
H9a .46854 .89202 .79270 .05000 1.00000 Uiso
H10a .44219 .77383 .87608 .05000 1.00000 Uiso
H11a .30464 .68027 .88531 .05000 1.00000 Uiso
H12a .18814 .69290 .81117 .05000 1.00000 Uiso
H16a .48797 .84251 .36195 .05000 1.00000 Uiso
H17a .46870 .72063 .27827 .05000 1.00000 Uiso
H18a .33318 .62018 .26510 .05000 1.00000 Uiso
H19a .21442 .63293 .33503 .05000 1.00000 Uiso
H211a .42023 1.03717 .71515 .05000 1.00000 Uiso
H212a .45577 .93982 .67127 .05000 1.00000 Uiso
H213a .38006 1.02395 .64656 .05000 1.00000 Uiso
H221a .47195 .90275 .47066 .05000 1.00000 Uiso
H222a .42327 1.00390 .43438 .05000 1.00000 Uiso
H223a .39528 .97188 .50337 .05000 1.00000 Uiso
H02b .31055 .30898 .54406 .05000 1.00000 Uiso
H04b .31907 .28610 .33337 .05000 1.00000 Uiso
H011b .27943 .34826 .43657 .05000 1.00000 Uiso
H012b .23677 .47743 .42761 .05000 1.00000 Uiso
H2b .10932 .40350 .37508 .05000 1.00000 Uiso
H31b .10493 .21914 .34545 .05000 1.00000 Uiso
H32b .20079 .19384 .38661 .05000 1.00000 Uiso
H41b .02835 .26918 .43253 .05000 1.00000 Uiso
H42b .07461 .14194 .44187 .05000 1.00000 Uiso
H51b .09341 .25761 .52901 .05000 1.00000 Uiso
H52b .19321 .21472 .50011 .05000 1.00000 Uiso
H6b .10782 .42815 .48172 .05000 1.00000 Uiso
H9b .21649 .62154 .67568 .05000 1.00000 Uiso
H10b .35139 .60334 .73677 .05000 1.00000 Uiso
H11b .46281 .47358 .71210 .05000 1.00000 Uiso
H12b .44585 .35495 .62662 .05000 1.00000 Uiso
H16b .21563 .53873 .16914 .05000 1.00000 Uiso
H17b .34927 .50504 .11430 .05000 1.00000 Uiso
H18b .46277 .38827 .15215 .05000 1.00000 Uiso
H19b .44800 .29802 .24740 .05000 1.00000 Uiso
H211b .10887 .59564 .60956 .05000 1.00000 Uiso
H212b .11560 .60108 .53744 .05000 1.00000 Uiso
H213b .06003 .50078 .56839 .05000 1.00000 Uiso
H221b .11310 .54396 .23721 .05000 1.00000 Uiso
H222b .06118 .44142 .26943 .05000 1.00000 Uiso
H223b .10226 .54095 .31080 .05000 1.00000 Uiso
H021 .51511 .68200 .58013 .05000 1.00000 Uiso
H022 .54462 .69305 .51012 .05000 1.00000 Uiso
H023 .54329 .57303 .54237 .05000 1.00000 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 .0319(10) .0506(12) .0446(12) -.0101(9) .0061(9) -.0093(10)
Cl2 .0350(10) .0515(13) .0521(12) -.0118(10) -.0095(9) .0093(11)
Cl3 .0453(11) .0336(11) .0611(13) .0051(10) .0035(10) -.0061(10)
Cl4 .0728(15) .0647(16) .0764(16) .0249(13) -.0214(13) -.0115(13)
N1a .026(4) .036(4) .030(4) -.005(3) -.001(3) .001(3)
N2a .027(3) .030(4) .028(4) -.005(3) -.002(3) .001(3)
N3a .027(4) .026(4) .033(4) -.006(3) .007(3) -.004(3)
N4a .028(4) .037(4) .033(4) -.007(3) -.001(3) .003(3)
C1a .028(4) .033(5) .025(4) -.003(4) -.002(3) -.004(4)
C2a .023(4) .038(5) .027(4) .003(4) .002(3) .000(4)
C3a .021(4) .038(5) .037(5) .002(4) -.002(4) -.000(4)
C4a .026(4) .044(5) .032(5) .001(4) .002(4) .000(4)
C5a .032(4) .042(5) .032(4) .007(4) .003(4) -.004(4)
C6a .027(4) .031(5) .027(4) .002(4) -.005(4) -.002(4)
C7a .022(4) .025(4) .031(4) .004(4) -.002(4) -.004(4)
C8a .037(5) .030(5) .025(4) .001(4) .002(4) .001(4)
C9a .024(4) .046(5) .034(5) -.007(4) -.004(4) .000(4)
C10a .038(5) .042(5) .031(5) .002(4) -.006(4) .006(4)
C11a .047(5) .034(5) .030(4) -.003(4) -.006(4) .007(4)
C12a .037(4) .040(5) .026(4) -.010(4) -.001(4) .005(4)
C13a .022(4) .031(5) .031(5) -.001(4) .000(4) -.003(4)
C14a .032(4) .023(4) .025(4) -.002(4) -.002(4) .000(4)
C15a .030(4) .031(5) .023(4) -.006(4) .004(4) -.001(4)
C16a .040(5) .029(5) .040(5) -.005(4) .005(4) .002(4)
C17a .044(5) .043(5) .038(5) .005(4) .010(4) -.005(4)
C18a .051(5) .045(6) .035(5) -.002(5) .002(4) -.012(4)
C19a .051(5) .037(5) .037(5) -.008(4) -.006(4) -.010(4)
C20a .030(4) .030(5) .030(5) -.001(4) .001(4) .004(4)
C21a .029(4) .054(6) .038(5) -.006(4) -.001(4) .010(4)
C22a .029(4) .046(5) .048(5) -.014(4) .003(4) -.017(4)
N1b .035(4) .025(4) .026(4) .008(3) -.003(3) -.006(3)
N2b .040(4) .032(4) .030(4) .009(3) -.006(3) -.008(3)
N3b .039(4) .029(4) .025(4) -.006(3) -.002(3) -.002(3)
N4b .037(4) .045(4) .043(4) .007(4) .004(3) .011(4)
C1b .047(5) .032(5) .026(4) -.007(4) .001(4) .000(4)
C2b .029(4) .037(5) .022(4) .008(4) .003(3) .000(4)
C3b .037(5) .041(5) .030(4) -.007(4) -.000(4) -.003(4)
C4b .042(5) .038(5) .040(5) -.008(4) -.003(4) -.003(4)
C5b .045(5) .035(5) .025(4) -.011(4) -.000(4) -.000(4)
C6b .034(4) .032(5) .028(4) -.000(4) .001(4) .000(4)
C7b .041(5) .022(5) .033(5) .001(4) -.002(4) .001(4)
C8b .034(5) .031(5) .032(5) -.001(4) .001(4) .001(4)
C9b .039(5) .038(5) .044(5) .002(4) -.004(4) -.004(4)
C10b .064(6) .041(5) .031(5) -.001(5) -.006(4) -.015(4)
C11b .054(6) .041(6) .057(6) .007(5) -.021(5) -.015(5)
C12b .042(5) .044(6) .051(5) .005(4) -.009(4) -.007(5)
C13b .036(5) .030(5) .033(5) .001(4) -.001(4) -.004(4)
C14b .030(5) .033(5) .033(5) -.001(4) -.003(4) -.004(4)
C15b .041(5) .035(5) .022(5) -.008(4) .002(4) -.001(4)
C16b .057(5) .037(5) .033(5) -.012(4) .007(4) -.011(4)
C17b .075(6) .037(6) .040(5) -.009(5) .024(5) -.011(4)
C18b .059(6) .061(7) .064(6) -.011(5) .038(5) -.014(6)
C19b .040(5) .056(6) .059(6) .007(5) .012(5) -.008(5)
C20b .037(5) .044(5) .031(5) -.002(4) .007(4) -.003(4)
C21b .038(5) .036(5) .046(5) .008(4) -.001(4) -.004(4)
C22b .034(5) .039(5) .044(5) -.001(4) -.004(4) .003(4)
C01 .086(8) .049(7) .081(7) -.020(7) .014(7) .007(6)
C02 .087(9) .121(11) .188(13) -.032(8) .007(9) -.059(10)
N01 .084(7) .099(8) .119(8) -.009(6) -.013(6) .056(6)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
N1a C7a . . 1.350(8)
N1a C8a . . 1.387(8)
N1a C21a . . 1.473(9)
N2a C7a . . 1.329(8)
N2a C13a . . 1.400(8)
N3a C14a . . 1.331(8)
N3a C15a . . 1.392(8)
N3a C22a . . 1.468(9)
N4a C14a . . 1.337(8)
N4a C20a . . 1.376(8)
C1a C2a . . 1.548(9)
C1a C6a . . 1.544(9)
C2a C3a . . 1.544(8)
C2a C14a . . 1.497(9)
C3a C4a . . 1.529(9)
C4a C5a . . 1.529(9)
C5a C6a . . 1.552(9)
C6a C7a . . 1.490(9)
C8a C9a . . 1.408(9)
C8a C13a . . 1.384(9)
C9a C10a . . 1.372(10)
C10a C11a . . 1.398(10)
C11a C12a . . 1.376(9)
C12a C13a . . 1.393(9)
C15a C16a . . 1.386(9)
C15a C20a . . 1.381(9)
C16a C17a . . 1.382(10)
C17a C18a . . 1.411(10)
C18a C19a . . 1.369(10)
C19a C20a . . 1.396(10)
N1b C7b . . 1.326(8)
N1b C8b . . 1.411(8)
N1b C21b . . 1.472(8)
N2b C7b . . 1.333(9)
N2b C13b . . 1.388(8)
N3b C14b . . 1.340(9)
N3b C15b . . 1.387(8)
N3b C22b . . 1.477(9)
N4b C14b . . 1.342(9)
N4b C20b . . 1.373(9)
C1b C2b . . 1.547(9)
C1b C6b . . 1.538(9)
C2b C3b . . 1.526(10)
C2b C14b . . 1.483(9)
C3b C4b . . 1.524(9)
C4b C5b . . 1.545(9)
C5b C6b . . 1.544(10)
C6b C7b . . 1.495(9)
C8b C9b . . 1.386(10)
C8b C13b . . 1.373(9)
C9b C10b . . 1.399(10)
C10b C11b . . 1.396(11)
C11b C12b . . 1.386(11)
C12b C13b . . 1.398(10)
C15b C16b . . 1.393(10)
C15b C20b . . 1.387(10)
C16b C17b . . 1.373(11)
C17b C18b . . 1.399(12)
C18b C19b . . 1.395(12)
C19b C20b . . 1.386(10)
C01 C02 . . 1.422(15)
C01 N01 . . 1.101(14)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
C7a N1a C8a . . . 109.1(5)
C7a N1a C21a . . . 127.2(6)
C8a N1a C21a . . . 123.8(5)
C7a N2a C13a . . . 109.4(5)
C14a N3a C15a . . . 109.0(5)
C14a N3a C22a . . . 127.4(6)
C15a N3a C22a . . . 123.6(5)
C14a N4a C20a . . . 109.1(5)
C2a C1a C6a . . . 108.7(5)
C1a C2a C3a . . . 110.1(5)
C1a C2a C14a . . . 112.5(6)
C3a C2a C14a . . . 112.5(5)
C2a C3a C4a . . . 109.4(5)
C3a C4a C5a . . . 111.0(6)
C4a C5a C6a . . . 110.2(5)
C1a C6a C5a . . . 111.2(5)
C1a C6a C7a . . . 109.7(5)
C5a C6a C7a . . . 111.0(5)
N1a C7a N2a . . . 108.6(6)
N1a C7a C6a . . . 125.6(6)
N2a C7a C6a . . . 125.8(6)
N1a C8a C9a . . . 132.0(6)
N1a C8a C13a . . . 106.7(6)
C9a C8a C13a . . . 121.3(6)
C8a C9a C10a . . . 116.5(6)
C9a C10a C11a . . . 121.2(6)
C10a C11a C12a . . . 123.3(6)
C11a C12a C13a . . . 115.2(6)
N2a C13a C8a . . . 106.2(6)
N2a C13a C12a . . . 131.3(6)
C8a C13a C12a . . . 122.5(6)
N3a C14a N4a . . . 108.8(6)
N3a C14a C2a . . . 125.3(6)
N4a C14a C2a . . . 125.9(6)
N3a C15a C16a . . . 131.5(6)
N3a C15a C20a . . . 106.1(6)
C16a C15a C20a . . . 122.4(6)
C15a C16a C17a . . . 116.9(6)
C16a C17a C18a . . . 120.4(7)
C17a C18a C19a . . . 122.7(7)
C18a C19a C20a . . . 116.4(7)
N4a C20a C15a . . . 107.0(6)
N4a C20a C19a . . . 131.7(6)
C15a C20a C19a . . . 121.3(6)
C7b N1b C8b . . . 108.6(5)
C7b N1b C21b . . . 126.3(6)
C8b N1b C21b . . . 125.1(5)
C7b N2b C13b . . . 109.2(6)
C14b N3b C15b . . . 109.5(6)
C14b N3b C22b . . . 125.1(6)
C15b N3b C22b . . . 125.3(6)
C14b N4b C20b . . . 109.7(6)
C2b C1b C6b . . . 109.7(5)
C1b C2b C3b . . . 110.9(5)
C1b C2b C14b . . . 111.2(5)
C3b C2b C14b . . . 111.6(6)
C2b C3b C4b . . . 110.7(6)
C3b C4b C5b . . . 111.6(6)
C4b C5b C6b . . . 111.1(6)
C1b C6b C5b . . . 111.1(6)
C1b C6b C7b . . . 110.2(5)
C5b C6b C7b . . . 110.2(6)
N1b C7b N2b . . . 109.2(6)
N1b C7b C6b . . . 126.2(6)
N2b C7b C6b . . . 124.5(6)
N1b C8b C9b . . . 131.0(6)
N1b C8b C13b . . . 106.2(6)
C9b C8b C13b . . . 122.8(6)
C8b C9b C10b . . . 115.6(7)
C9b C10b C11b . . . 121.4(7)
C10b C11b C12b . . . 122.5(7)
C11b C12b C13b . . . 115.4(7)
N2b C13b C8b . . . 106.7(6)
N2b C13b C12b . . . 131.0(6)
C8b C13b C12b . . . 122.3(6)
N3b C14b N4b . . . 107.9(6)
N3b C14b C2b . . . 127.6(6)
N4b C14b C2b . . . 124.5(6)
N3b C15b C16b . . . 131.5(6)
N3b C15b C20b . . . 106.1(6)
C16b C15b C20b . . . 122.3(6)
C15b C16b C17b . . . 116.3(7)
C16b C17b C18b . . . 122.1(7)
C17b C18b C19b . . . 121.3(8)
C18b C19b C20b . . . 116.6(7)
N4b C20b C15b . . . 106.8(6)
N4b C20b C19b . . . 131.8(7)
C15b C20b C19b . . . 121.4(7)
C02 C01 N01 . . . 178.9(11)

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
C8a N1a C7a N2a . . . . .8(7)
C8a N1a C7a C6a . . . . -176.5(6)
C21a N1a C7a N2a . . . . -178.2(6)
C21a N1a C7a C6a . . . . 4.5(10)
C7a N1a C8a C9a . . . . 179.2(7)
C7a N1a C8a C13a . . . . -.4(7)
C21a N1a C8a C9a . . . . -1.8(11)
C21a N1a C8a C13a . . . . 178.6(6)
C13a N2a C7a N1a . . . . -.9(7)
C13a N2a C7a C6a . . . . 176.4(6)
C7a N2a C13a C8a . . . . .7(7)
C7a N2a C13a C12a . . . . -179.9(7)
C15a N3a C14a N4a . . . . 1.5(7)
C15a N3a C14a C2a . . . . -175.9(6)
C22a N3a C14a N4a . . . . -179.8(6)
C22a N3a C14a C2a . . . . 2.8(10)
C14a N3a C15a C16a . . . . 176.6(7)
C14a N3a C15a C20a . . . . -.6(7)
C22a N3a C15a C16a . . . . -2.1(11)
C22a N3a C15a C20a . . . . -179.3(6)
C20a N4a C14a N3a . . . . -1.9(7)
C20a N4a C14a C2a . . . . 175.5(6)
C14a N4a C20a C15a . . . . 1.5(7)
C14a N4a C20a C19a . . . . -176.6(7)
C6a C1a C2a C3a . . . . -59.7(7)
C6a C1a C2a C14a . . . . 174.1(5)
C2a C1a C6a C5a . . . . 57.5(7)
C2a C1a C6a C7a . . . . -179.3(5)
C1a C2a C3a C4a . . . . 60.7(7)
C14a C2a C3a C4a . . . . -173.0(6)
C1a C2a C14a N3a . . . . -81.7(8)
C1a C2a C14a N4a . . . . 101.3(7)
C3a C2a C14a N3a . . . . 153.4(6)
C3a C2a C14a N4a . . . . -23.6(9)
C2a C3a C4a C5a . . . . -59.2(7)
C3a C4a C5a C6a . . . . 56.9(7)
C4a C5a C6a C1a . . . . -56.4(7)
C4a C5a C6a C7a . . . . -178.9(6)
C1a C6a C7a N1a . . . . 83.1(8)
C1a C6a C7a N2a . . . . -93.7(7)
C5a C6a C7a N1a . . . . -153.5(6)
C5a C6a C7a N2a . . . . 29.6(9)
N1a C8a C9a C10a . . . . -179.7(7)
C13a C8a C9a C10a . . . . -.2(10)
N1a C8a C13a N2a . . . . -.2(7)
N1a C8a C13a C12a . . . . -179.6(6)
C9a C8a C13a N2a . . . . -179.8(6)
C9a C8a C13a C12a . . . . .8(10)
C8a C9a C10a C11a . . . . -.4(10)
C9a C10a C11a C12a . . . . .5(11)
C10a C11a C12a C13a . . . . .0(10)
C11a C12a C13a N2a . . . . -180.0(7)
C11a C12a C13a C8a . . . . -.7(10)
N3a C15a C16a C17a . . . . -176.8(7)
C20a C15a C16a C17a . . . . -.0(10)
N3a C15a C20a N4a . . . . -.6(7)
N3a C15a C20a C19a . . . . 177.8(6)
C16a C15a C20a N4a . . . . -178.1(6)
C16a C15a C20a C19a . . . . .3(10)
C15a C16a C17a C18a . . . . .2(10)
C16a C17a C18a C19a . . . . -.8(11)
C17a C18a C19a C20a . . . . 1.0(11)
C18a C19a C20a N4a . . . . 177.1(7)
C18a C19a C20a C15a . . . . -.8(10)
C8b N1b C7b N2b . . . . -.5(7)
C8b N1b C7b C6b . . . . -177.9(6)
C21b N1b C7b N2b . . . . -179.6(6)
C21b N1b C7b C6b . . . . 3.0(10)
C7b N1b C8b C9b . . . . -179.0(7)
C7b N1b C8b C13b . . . . -.4(7)
C21b N1b C8b C9b . . . . .2(11)
C21b N1b C8b C13b . . . . 178.8(6)
C13b N2b C7b N1b . . . . 1.1(8)
C13b N2b C7b C6b . . . . 178.6(6)
C7b N2b C13b C8b . . . . -1.3(8)
C7b N2b C13b C12b . . . . -179.4(7)
C15b N3b C14b N4b . . . . .5(8)
C15b N3b C14b C2b . . . . -179.8(7)
C22b N3b C14b N4b . . . . 177.6(6)
C22b N3b C14b C2b . . . . -2.7(11)
C14b N3b C15b C16b . . . . -176.8(7)
C14b N3b C15b C20b . . . . -.7(8)
C22b N3b C15b C16b . . . . 6.1(11)
C22b N3b C15b C20b . . . . -177.8(6)
C20b N4b C14b N3b . . . . -.1(8)
C20b N4b C14b C2b . . . . -179.8(6)
C14b N4b C20b C15b . . . . -.4(8)
C14b N4b C20b C19b . . . . 178.1(8)
C6b C1b C2b C3b . . . . -58.5(7)
C6b C1b C2b C14b . . . . 176.7(6)
C2b C1b C6b C5b . . . . 56.6(7)
C2b C1b C6b C7b . . . . 179.0(6)
C1b C2b C3b C4b . . . . 58.3(7)
C14b C2b C3b C4b . . . . -177.1(5)
C1b C2b C14b N3b . . . . -119.2(7)
C1b C2b C14b N4b . . . . 60.5(9)
C3b C2b C14b N3b . . . . 116.4(7)
C3b C2b C14b N4b . . . . -63.9(8)
C2b C3b C4b C5b . . . . -56.0(7)
C3b C4b C5b C6b . . . . 54.3(7)
C4b C5b C6b C1b . . . . -54.8(7)
C4b C5b C6b C7b . . . . -177.2(6)
C1b C6b C7b N1b . . . . 119.6(7)
C1b C6b C7b N2b . . . . -57.4(9)
C5b C6b C7b N1b . . . . -117.4(7)
C5b C6b C7b N2b . . . . 65.6(8)
N1b C8b C9b C10b . . . . -179.8(7)
C13b C8b C9b C10b . . . . 1.8(10)
N1b C8b C13b N2b . . . . 1.0(7)
N1b C8b C13b C12b . . . . 179.2(6)
C9b C8b C13b N2b . . . . 179.8(6)
C9b C8b C13b C12b . . . . -2.0(11)
C8b C9b C10b C11b . . . . -.3(11)
C9b C10b C11b C12b . . . . -.9(12)
C10b C11b C12b C13b . . . . .8(11)
C11b C12b C13b N2b . . . . 178.4(7)
C11b C12b C13b C8b . . . . .6(10)
N3b C15b C16b C17b . . . . 177.5(7)
C20b C15b C16b C17b . . . . 1.9(10)
N3b C15b C20b N4b . . . . .7(8)
N3b C15b C20b C19b . . . . -178.0(7)
C16b C15b C20b N4b . . . . 177.2(7)
C16b C15b C20b C19b . . . . -1.5(11)
C15b C16b C17b C18b . . . . -1.1(11)
C16b C17b C18b C19b . . . . -.2(13)
C17b C18b C19b C20b . . . . .7(12)
C18b C19b C20b N4b . . . . -178.2(8)
C18b C19b C20b C15b . . . . .1(11)

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2a H02a Cl1 . . . 1.06 1.93 2.978(5) 168
N4a H04a Cl2 . . . 1.00 2.09 3.020(5) 154
N2b H02b Cl3 . . . 0.91 2.16 3.020(6) 156
N4b H04b Cl4 . . 3_666 0.86 2.15 2.978(6) 162

#=END==============================================================

# Attachment '3bH2Mn.cif'

data_3bH2Mn
_database_code_depnum_ccdc_archive 'CCDC 602152'
#--(C22H26N4)(MnCl4).(H2 O)---------------------------- [3bH2][MnCl4]H2O ---
_audit_creation_date             2004-02-04
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2005-12-05
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1

_chemical_formula_moiety         'C22 H26 N4 , Cl4 Mn , H2 O'
_chemical_formula_sum            'C22 H28 Cl4 Mn N4 O'
_chemical_formula_weight         561.3

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
_cell_length_a                   9.5492(8)
_cell_length_b                   9.8088(9)
_cell_length_c                   14.7179(13)
_cell_angle_alpha                84.185(10)
_cell_angle_beta                 86.801(10)
_cell_angle_gamma                65.969(9)
_cell_volume                     1252.4(2)
_cell_formula_units_Z            2
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      not_measured
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      3.7
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200
_exptl_crystal_F_000             578
_exptl_absorpt_coefficient_mu    .98
_exptl_crystal_description       prism
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .11
_exptl_crystal_colour            colorless

_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_detector_area_resol_mean 6
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED; Stoe & Cie, 1999'
_exptl_absorpt_correction_T_min  .8303
_exptl_absorpt_correction_T_max  .9151
_diffrn_reflns_number            19221
_reflns_number_total             5601
_reflns_number_gt                3418
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        27.5
_diffrn_measured_fraction_theta_max 1.
_diffrn_measured_fraction_theta_full 1.
_diffrn_reflns_av_R_equivalents  .046
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_decay_%        0
_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .029
_refine_ls_wR_factor_ref         .030
_refine_ls_goodness_of_fit_ref   1.17
_refine_ls_number_reflns         3557
_refine_ls_number_parameters     301
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.0001(Fo^2^)]
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          .0016
_refine_diff_density_max         .539
_refine_diff_density_min         -.534
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .00000
_refine_ls_abs_structure_details none
_refine_special_details          
;
Hydrogen treatment:
- For the methyl groups: calculated and refined with restraints
on bond lengths and bond angles and blocked in the last cylcles.
- For H2O : observed and refined with restraints on bond lengths
and bond angles (fixed Uiso).
- For -NH: observed and refined without restraint (fixed Uiso)
- Other H atoms: calculated.
;
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_structure_solution    SIR97
_computing_structure_refinement  xtal_CRYLSQ
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO

loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003
O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006
Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .132 .159
Mn Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .295 .729

loop_
_atom_site_label
_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
N1 .1355(3) .2124(3) .43494(14) .0260(18) 1.00000 Uani
N2 -.1021(3) .3174(3) .48263(13) .0241(17) 1.00000 Uani
N3 .1936(3) -.0812(3) .07804(13) .0255(18) 1.00000 Uani
N4 .1538(3) .1524(3) .04409(13) .0240(17) 1.00000 Uani
C1 -.0631(3) .1943(3) .33596(15) .026(3) 1.00000 Uani
C2 .0587(3) .1507(3) .25840(16) .025(2) 1.00000 Uani
C3 -.0032(3) .1010(3) .17786(16) .025(2) 1.00000 Uani
C4 -.0490(3) -.0282(3) .21038(16) .027(3) 1.00000 Uani
C5 -.1676(4) .0164(3) .28781(17) .030(3) 1.00000 Uani
C6 -.1076(4) .0625(3) .36759(16) .030(3) 1.00000 Uani
C7 -.0094(3) .2426(3) .41572(15) .024(2) 1.00000 Uani
C8 .1394(4) .2701(3) .51758(15) .025(3) 1.00000 Uani
C9 .2608(4) .2715(3) .56561(17) .030(3) 1.00000 Uani
C10 .2209(4) .3398(3) .64702(17) .032(3) 1.00000 Uani
C11 .0687(4) .4041(3) .67814(16) .032(3) 1.00000 Uani
C12 -.0515(4) .4047(3) .62978(16) .028(3) 1.00000 Uani
C13 -.0112(3) .3355(3) .54777(15) .023(2) 1.00000 Uani
C14 .1138(3) .0584(3) .10103(15) .024(2) 1.00000 Uani
C15 .2921(3) -.0796(3) .00425(15) .024(2) 1.00000 Uani
C16 .3972(4) -.1952(3) -.04322(17) .032(3) 1.00000 Uani
C17 .4783(4) -.1513(4) -.11279(17) .036(3) 1.00000 Uani
C18 .4537(4) -.0007(4) -.13392(17) .035(3) 1.00000 Uani
C19 .3471(4) .1132(3) -.08736(16) .031(3) 1.00000 Uani
C20 .2666(3) .0697(3) -.01715(15) .023(2) 1.00000 Uani
C21 -.2712(4) .3733(4) .48826(18) .035(3) 1.00000 Uani
C22 .0874(4) .3170(3) .04037(18) .033(3) 1.00000 Uani
Mn .45216(5) .53954(5) .22355(3) .0239(4) 1.00000 Uani
Cl1 .24289(8) .58023(7) .12827(5) .0329(6) 1.00000 Uani
Cl2 .46701(8) .34361(7) .33637(4) .0313(6) 1.00000 Uani
Cl3 .37547(8) .76898(7) .29364(5) .0330(6) 1.00000 Uani
Cl4 .69257(8) .48931(8) .15249(5) .0342(6) 1.00000 Uani
O1w .4145(3) .0448(3) .37056(16) .050(3) 1.00000 Uani
H1 -.15320 .27950 .31106 .04000 1.00000 Uiso
H21 .08154 .23736 .23670 .04000 1.00000 Uiso
H22 .15212 .06806 .28137 .04000 1.00000 Uiso
H3 -.09615 .18613 .15546 .04000 1.00000 Uiso
H41 -.09210 -.05428 .15914 .04000 1.00000 Uiso
H42 .04223 -.11531 .23229 .04000 1.00000 Uiso
H51 -.26021 .10049 .26442 .04000 1.00000 Uiso
H52 -.19320 -.06932 .30829 .04000 1.00000 Uiso
H61 -.18655 .09230 .41554 .04000 1.00000 Uiso
H62 -.01630 -.02302 .39205 .04000 1.00000 Uiso
H01 .224(4) .156(4) .4082(19) .04000 1.00000 Uiso
H9 .36737 .22698 .54379 .04000 1.00000 Uiso
H10 .30149 .34385 .68358 .04000 1.00000 Uiso
H11 .04697 .44945 .73655 .04000 1.00000 Uiso
H12 -.15842 .45081 .65114 .04000 1.00000 Uiso
H03 .188(4) -.160(4) .1048(19) .04000 1.00000 Uiso
H16 .41356 -.30028 -.02867 .04000 1.00000 Uiso
H17 .55508 -.22767 -.14821 .04000 1.00000 Uiso
H18 .51430 .02422 -.18355 .04000 1.00000 Uiso
H19 .32957 .21840 -.10303 .04000 1.00000 Uiso
H211 -.30053 .30674 .52914 .04000 1.00000 Uiso
H212 -.31398 .47312 .51057 .04000 1.00000 Uiso
H213 -.31053 .37935 .42914 .04000 1.00000 Uiso
H221 -.00233 .35109 .07836 .04000 1.00000 Uiso
H222 .16086 .34887 .06137 .04000 1.00000 Uiso
H223 .06163 .35791 -.02139 .04000 1.00000 Uiso
H1w .438(4) -.035(3) .3429(16) .04000 1.00000 Uiso
H2w .458(4) .098(3) .3435(16) .04000 1.00000 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 .0267(14) .0236(11) .0249(11) -.0068(11) .0053(10) -.0071(9)
N2 .0245(13) .0254(11) .0220(10) -.0095(10) -.0009(9) -.0031(9)
N3 .0372(15) .0184(11) .0213(10) -.0116(11) -.0014(9) -.0015(8)
N4 .0326(14) .0163(10) .0221(10) -.0084(10) -.0044(9) -.0017(8)
C1 .0306(17) .0205(12) .0237(12) -.0082(12) -.0027(11) -.0023(10)
C2 .0310(16) .0205(12) .0250(12) -.0109(12) -.0020(11) -.0023(10)
C3 .0274(16) .0206(12) .0233(12) -.0046(12) -.0032(11) -.0031(10)
C4 .0280(16) .0232(13) .0301(13) -.0091(12) -.0053(11) -.0056(10)
C5 .0309(17) .0260(14) .0357(14) -.0135(13) -.0001(12) -.0043(11)
C6 .0356(18) .0308(15) .0264(13) -.0160(14) .0010(12) -.0046(11)
C7 .0261(16) .0185(12) .0253(12) -.0076(12) .0007(11) -.0015(10)
C8 .0307(17) .0205(12) .0220(12) -.0095(12) .0006(11) -.0040(10)
C9 .0261(17) .0278(14) .0354(14) -.0091(13) -.0018(12) -.0036(11)
C10 .0345(18) .0313(15) .0329(14) -.0149(14) -.0073(12) -.0033(12)
C11 .044(2) .0287(14) .0251(13) -.0162(14) -.0014(12) -.0060(11)
C12 .0306(17) .0237(13) .0277(13) -.0094(13) .0027(11) -.0058(10)
C13 .0288(17) .0187(12) .0225(12) -.0102(12) -.0029(11) -.0000(10)
C14 .0312(16) .0203(12) .0201(11) -.0096(12) -.0064(10) -.0007(10)
C15 .0308(16) .0230(13) .0197(11) -.0105(12) -.0043(11) -.0025(10)
C16 .0423(19) .0258(14) .0291(13) -.0139(14) -.0006(12) -.0086(11)
C17 .0385(19) .0410(16) .0296(14) -.0145(15) .0040(12) -.0178(12)
C18 .0416(19) .0449(17) .0245(13) -.0240(16) .0014(12) -.0046(12)
C19 .0403(18) .0318(15) .0269(13) -.0203(14) -.0043(12) .0003(11)
C20 .0284(16) .0223(13) .0196(11) -.0099(12) -.0048(10) -.0039(10)
C21 .0337(18) .0399(16) .0312(14) -.0127(14) .0021(12) -.0095(12)
C22 .0396(19) .0185(13) .0401(15) -.0096(13) -.0000(13) -.0023(11)
Mn .0234(3) .0202(2) .0276(2) -.00744(18) -.00133(16) -.00452(15)
Cl1 .0385(5) .0245(4) .0381(4) -.0139(4) -.0135(3) -.0010(3)
Cl2 .0328(4) .0254(4) .0315(4) -.0080(3) .0003(3) -.0003(3)
Cl3 .0316(5) .0246(4) .0431(4) -.0095(3) .0008(3) -.0131(3)
Cl4 .0294(5) .0285(4) .0416(4) -.0089(4) .0086(3) -.0068(3)
O1w .0437(15) .0407(13) .0693(15) -.0194(12) .0157(11) -.0252(11)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
N1 C7 . . 1.332(4)
N1 C8 . . 1.401(4)
N1 H01 . . .89(3)
N2 C7 . . 1.347(3)
N2 C13 . . 1.399(4)
N2 C21 . . 1.479(4)
N3 C14 . . 1.337(3)
N3 C15 . . 1.399(4)
N3 H03 . . .85(4)
N4 C14 . . 1.339(4)
N4 C20 . . 1.400(3)
N4 C22 . . 1.471(4)
C1 C2 . . 1.544(4)
C1 C6 . . 1.540(5)
C1 C7 . . 1.498(4)
C2 C3 . . 1.556(4)
C3 C4 . . 1.527(5)
C3 C14 . . 1.508(4)
C4 C5 . . 1.525(4)
C5 C6 . . 1.518(5)
C8 C9 . . 1.397(5)
C8 C13 . . 1.382(4)
C9 C10 . . 1.390(4)
C10 C11 . . 1.400(4)
C11 C12 . . 1.381(5)
C12 C13 . . 1.403(4)
C15 C16 . . 1.392(4)
C15 C20 . . 1.389(4)
C16 C17 . . 1.388(5)
C17 C18 . . 1.402(5)
C18 C19 . . 1.381(4)
C19 C20 . . 1.389(4)
Mn Cl1 . . 2.3810(9)
Mn Cl2 . . 2.3724(8)
Mn Cl3 . . 2.3894(8)
Mn Cl4 . . 2.3499(9)
O1w H1w . . .86(3)
O1w H2w . . .85(3)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
C7 N1 C8 . . . 109.3(3)
C7 N1 H01 . . . 131(3)
C8 N1 H01 . . . 119(3)
C7 N2 C13 . . . 108.2(3)
C7 N2 C21 . . . 127.1(3)
C13 N2 C21 . . . 124.7(2)
C14 N3 C15 . . . 109.7(3)
C14 N3 H03 . . . 125.6(18)
C15 N3 H03 . . . 124.7(18)
C14 N4 C20 . . . 109.0(2)
C14 N4 C22 . . . 127.2(2)
C20 N4 C22 . . . 123.6(3)
C2 C1 C6 . . . 110.3(3)
C2 C1 C7 . . . 112.2(3)
C6 C1 C7 . . . 109.8(2)
C1 C2 C3 . . . 109.8(3)
C2 C3 C4 . . . 110.8(2)
C2 C3 C14 . . . 110.8(3)
C4 C3 C14 . . . 110.9(3)
C3 C4 C5 . . . 110.3(3)
C4 C5 C6 . . . 111.5(3)
C1 C6 C5 . . . 110.2(2)
N1 C7 N2 . . . 109.2(3)
N1 C7 C1 . . . 126.4(3)
N2 C7 C1 . . . 124.3(3)
N1 C8 C9 . . . 131.7(3)
N1 C8 C13 . . . 106.1(3)
C9 C8 C13 . . . 122.3(3)
C8 C9 C10 . . . 115.7(3)
C9 C10 C11 . . . 122.0(3)
C10 C11 C12 . . . 122.2(3)
C11 C12 C13 . . . 115.7(3)
N2 C13 C8 . . . 107.2(2)
N2 C13 C12 . . . 130.7(3)
C8 C13 C12 . . . 122.1(3)
N3 C14 N4 . . . 108.7(3)
N3 C14 C3 . . . 125.0(3)
N4 C14 C3 . . . 126.3(3)
N3 C15 C16 . . . 131.2(3)
N3 C15 C20 . . . 105.9(2)
C16 C15 C20 . . . 122.9(3)
C15 C16 C17 . . . 115.2(3)
C16 C17 C18 . . . 122.0(3)
C17 C18 C19 . . . 122.3(3)
C18 C19 C20 . . . 116.0(3)
N4 C20 C15 . . . 106.7(3)
N4 C20 C19 . . . 131.6(3)
C15 C20 C19 . . . 121.7(3)
Cl1 Mn Cl2 . . . 106.96(4)
Cl1 Mn Cl3 . . . 103.95(3)
Cl1 Mn Cl4 . . . 117.45(3)
Cl2 Mn Cl3 . . . 109.53(3)
Cl2 Mn Cl4 . . . 110.63(3)
Cl3 Mn Cl4 . . . 107.98(4)
H1w O1w H2w . . . 110(3)

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
C8 N1 C7 N2 . . . . -.3(3)
C8 N1 C7 C1 . . . . -176.9(3)
H01 N1 C7 N2 . . . . 172(3)
H01 N1 C7 C1 . . . . -5(3)
C7 N1 C8 C9 . . . . -178.1(3)
C7 N1 C8 C13 . . . . .6(3)
H01 N1 C8 C9 . . . . 9(3)
H01 N1 C8 C13 . . . . -173(3)
C13 N2 C7 N1 . . . . -.1(3)
C13 N2 C7 C1 . . . . 176.6(3)
C21 N2 C7 N1 . . . . 179.6(3)
C21 N2 C7 C1 . . . . -3.7(4)
C7 N2 C13 C8 . . . . .5(3)
C7 N2 C13 C12 . . . . -179.8(3)
C21 N2 C13 C8 . . . . -179.2(3)
C21 N2 C13 C12 . . . . .5(5)
C15 N3 C14 N4 . . . . 1.1(4)
C15 N3 C14 C3 . . . . -179.6(3)
H03 N3 C14 N4 . . . . 180(3)
H03 N3 C14 C3 . . . . 0(3)
C14 N3 C15 C16 . . . . 179.6(3)
C14 N3 C15 C20 . . . . -.6(4)
H03 N3 C15 C16 . . . . 0(3)
H03 N3 C15 C20 . . . . -179(3)
C20 N4 C14 N3 . . . . -1.2(4)
C20 N4 C14 C3 . . . . 179.5(3)
C22 N4 C14 N3 . . . . 175.5(3)
C22 N4 C14 C3 . . . . -3.7(5)
C14 N4 C20 C15 . . . . .9(3)
C14 N4 C20 C19 . . . . -178.5(3)
C22 N4 C20 C15 . . . . -176.1(3)
C22 N4 C20 C19 . . . . 4.6(5)
C6 C1 C2 C3 . . . . 57.0(3)
C7 C1 C2 C3 . . . . 179.75(19)
C2 C1 C6 C5 . . . . -57.9(3)
C7 C1 C6 C5 . . . . 177.96(19)
C2 C1 C7 N1 . . . . -19.6(4)
C2 C1 C7 N2 . . . . 164.4(3)
C6 C1 C7 N1 . . . . 103.4(3)
C6 C1 C7 N2 . . . . -72.6(3)
C1 C2 C3 C4 . . . . -56.8(3)
C1 C2 C3 C14 . . . . 179.75(19)
C2 C3 C4 C5 . . . . 56.8(3)
C14 C3 C4 C5 . . . . -179.8(3)
C2 C3 C14 N3 . . . . 108.9(4)
C2 C3 C14 N4 . . . . -72.0(4)
C4 C3 C14 N3 . . . . -14.5(4)
C4 C3 C14 N4 . . . . 164.6(3)
C3 C4 C5 C6 . . . . -57.9(3)
C4 C5 C6 C1 . . . . 58.3(3)
N1 C8 C9 C10 . . . . -179.9(3)
C13 C8 C9 C10 . . . . 1.5(4)
N1 C8 C13 N2 . . . . -.6(3)
N1 C8 C13 C12 . . . . 179.6(3)
C9 C8 C13 N2 . . . . 178.3(3)
C9 C8 C13 C12 . . . . -1.5(4)
C8 C9 C10 C11 . . . . -.6(4)
C9 C10 C11 C12 . . . . -.4(5)
C10 C11 C12 C13 . . . . .6(4)
C11 C12 C13 N2 . . . . -179.3(3)
C11 C12 C13 C8 . . . . .4(4)
N3 C15 C16 C17 . . . . -178.8(3)
C20 C15 C16 C17 . . . . 1.4(5)
N3 C15 C20 N4 . . . . -.2(3)
N3 C15 C20 C19 . . . . 179.3(3)
C16 C15 C20 N4 . . . . 179.6(3)
C16 C15 C20 C19 . . . . -.9(5)
C15 C16 C17 C18 . . . . -.8(5)
C16 C17 C18 C19 . . . . -.4(5)
C17 C18 C19 C20 . . . . .9(5)
C18 C19 C20 N4 . . . . 179.0(3)
C18 C19 C20 C15 . . . . -.3(5)

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H01 O1w . . . 0.89(3) 1.79(3) 2.677(3) 171(3)
N3 H03 Cl1 . . 1_545 0.85(3) 2.37(3) 3.172(2) 156(2)
O1w H1w Cl3 . . 1_545 0.86(2) 2.42(3) 3.199(3) 151(3)
O1w H2w Cl2 . . . 0.85(3) 2.43(3) 3.156(3) 143(2)
#==END================================================================
# Attachment '5aH3.cif'

data_5aH3
_database_code_depnum_ccdc_archive 'CCDC 602153'

#-- (C27H27N6)Cl3(CH3OH)2 ------------------------------ [5aH3]Cl3.2MeOH ---

_audit_creation_date             1999-04-22
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2005-12-05
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1

_chemical_formula_moiety         '(C27 H27 N6) , Cl3 , (C H4 O)2'
_chemical_formula_sum            'C29 H35 Cl3 N6 O2'
_chemical_formula_weight         606.0
_chemical_absolute_configuration ad

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,1/2+y,-z
_cell_length_a                   8.5221(7)
_cell_length_b                   11.8040(10)
_cell_length_c                   14.8840(10)
_cell_angle_alpha                90.00000
_cell_angle_beta                 95.929(7)
_cell_angle_gamma                90.00000
_cell_volume                     1489.2(2)
_cell_formula_units_Z            2
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      not_mesaured
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54183
_cell_measurement_reflns_used    26
_cell_measurement_theta_min      17.5
_cell_measurement_theta_max      24.5
_cell_measurement_temperature    200
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    3.088
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_exptl_crystal_colour            colorless

_diffrn_measurement_device_type  Stoe_Stadi-4_4-circle_diffractometer
_diffrn_measurement_method       \w-2\q_scans
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'xtal_lsabs (Flack & al. 1992)'
_exptl_absorpt_correction_T_min  .428439
_exptl_absorpt_correction_T_max  .715121
_diffrn_reflns_number            3845
_reflns_number_total             3624
_reflns_number_gt                3258
_reflns_Friedel_coverage         .94
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_diffrn_reflns_theta_max         54.5
_diffrn_reflns_theta_full        54.5
_diffrn_measured_fraction_theta_max 1.
_diffrn_measured_fraction_theta_full 1.
_diffrn_reflns_av_R_equivalents  .04
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_standards_number         2
_diffrn_standards_interval_time  45
_diffrn_standards_decay_%        0

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .051
_refine_ls_wR_factor_ref         .049
_refine_ls_goodness_of_fit_ref   2.47(4)
_refine_ls_number_reflns         3258
_refine_ls_number_parameters     386
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     \w=1/[\s^2(Fo)+0.0001(Fo^2)]
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          .0002
_refine_diff_density_max         .272
_refine_diff_density_min         -.248
_refine_ls_extinction_method     Zachariasen
_refine_ls_extinction_coef       1811(301)
_refine_ls_abs_structure_details Flack_xabs_refined
_refine_ls_abs_structure_Flack   0.01(3)

_refine_special_details          
;
Hydrogen treatment:
H (N-H and O-H): refined with a fixed value of Uiso
Other H atom : refined with restraint and fixed in the last cylces

Definition of polar origin:
y(Cl1) = fixed as a hard constraint
;

_computing_data_collection       Stoe_Stadi-4
_computing_cell_refinement       Xtal_latcon
_computing_data_reduction        xtal_REFCAL_LSABS__SORTRF
_computing_structure_solution    multan_87
_computing_structure_refinement  xtal_CRYLSQ
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO

loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .017 .009
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .047 .032
N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .029 .018
Cl Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .348 .702

loop_
_atom_site_label
_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
N1 .2606(9) .4332(7) .2416(5) .031(5) 1.00000 Uani
N2 .0422(9) .3667(7) .2829(5) .031(5) 1.00000 Uani
N3 -.1177(9) .5788(8) .5979(6) .027(5) 1.00000 Uani
N4 .0440(9) .5093(8) .7067(5) .029(5) 1.00000 Uani
N5 .5636(8) .3470(7) .6794(5) .030(5) 1.00000 Uani
N6 .6798(8) .3366(7) .5552(5) .027(5) 1.00000 Uani
C1 .2258(11) .4611(9) .4043(7) .024(6) 1.00000 Uani
C2 .0865(11) .4634(9) .4635(6) .027(6) 1.00000 Uani
C3 .1485(10) .5189(9) .5547(6) .027(6) 1.00000 Uani
C4 .2883(11) .4529(9) .6021(7) .027(5) 1.00000 Uani
C5 .4215(10) .4408(9) .5412(6) .030(6) 1.00000 Uani
C6 .3620(10) .3882(9) .4483(6) .027(5) 1.00000 Uani
C7 .1753(10) .4206(9) .3106(6) .028(6) 1.00000 Uani
C8 .1802(11) .3872(10) .1638(6) .032(6) 1.00000 Uani
C9 .2163(12) .3822(11) .0757(7) .043(7) 1.00000 Uani
C10 .1044(12) .3306(11) .0153(7) .051(8) 1.00000 Uani
C11 -.0368(11) .2881(13) .0412(7) .055(8) 1.00000 Uani
C12 -.0715(11) .2927(11) .1300(7) .045(7) 1.00000 Uani
C13 .0394(11) .3437(9) .1902(6) .032(6) 1.00000 Uani
C14 .0239(11) .5329(9) .6176(6) .027(6) 1.00000 Uani
C15 -.1941(10) .5869(9) .6768(6) .028(6) 1.00000 Uani
C16 -.3408(11) .6268(10) .6913(7) .036(6) 1.00000 Uani
C17 -.3823(12) .6182(10) .7788(7) .043(7) 1.00000 Uani
C18 -.2784(12) .5706(10) .8482(7) .042(7) 1.00000 Uani
C19 -.1317(12) .5325(9) .8334(7) .039(7) 1.00000 Uani
C20 -.0922(11) .5415(9) .7442(7) .032(6) 1.00000 Uani
C21 .5512(10) .3735(8) .5904(6) .026(6) 1.00000 Uani
C22 .7070(10) .2928(9) .7013(7) .029(6) 1.00000 Uani
C23 .7759(11) .2506(9) .7834(6) .031(6) 1.00000 Uani
C24 .9239(12) .2029(10) .7828(7) .039(7) 1.00000 Uani
C25 1.0022(11) .1964(10) .7035(7) .036(6) 1.00000 Uani
C26 .9309(10) .2383(8) .6228(7) .028(6) 1.00000 Uani
C27 .7831(10) .2853(9) .6230(6) .026(6) 1.00000 Uani
O1a .5265(8) .5534(7) .2368(5) .048(5) 1.00000 Uani
C1a .6478(13) .5098(12) .1868(8) .061(8) 1.00000 Uani
O1b .4145(10) .8170(10) .0228(6) .077(7) 1.00000 Uani
C1b .4582(16) .7080(15) .0041(10) .082(11) 1.00000 Uani
Cl1 .2539(3) .78000 .63894(15) .0348(14) 1.00000 Uani
Cl2 .3308(3) .1289(3) .57366(16) .0364(14) 1.00000 Uani
Cl3 .3267(3) .3941(4) .82526(17) .0538(17) 1.00000 Uani
H1 .27141 .54498 .39411 .05000 1.00000 Uiso
H21 -.01537 .51186 .43701 .05000 1.00000 Uiso
H22 .04355 .37971 .47321 .05000 1.00000 Uiso
H3 .19623 .60042 .53857 .05000 1.00000 Uiso
H41 .34029 .48916 .66423 .05000 1.00000 Uiso
H42 .24786 .37030 .61993 .05000 1.00000 Uiso
H5 .47057 .51998 .52062 .05000 1.00000 Uiso
H61 .46571 .39242 .41089 .05000 1.00000 Uiso
H62 .32999 .30139 .46033 .05000 1.00000 Uiso
H9 .33627 .40971 .06472 .05000 1.00000 Uiso
H10 .12236 .34320 -.05468 .05000 1.00000 Uiso
H11 -.12670 .25401 -.01024 .05000 1.00000 Uiso
H12 -.17414 .25211 .15429 .05000 1.00000 Uiso
H16 -.42611 .66376 .63925 .05000 1.00000 Uiso
H17 -.49794 .65400 .78677 .05000 1.00000 Uiso
H18 -.31801 .57279 .91437 .05000 1.00000 Uiso
H19 -.04961 .49743 .88622 .05000 1.00000 Uiso
H23 .71193 .24448 .84168 .05000 1.00000 Uiso
H24 .99799 .17716 .84187 .05000 1.00000 Uiso
H25 1.12348 .17070 .71173 .05000 1.00000 Uiso
H26 .98730 .22854 .56177 .05000 1.00000 Uiso
H11a .71857 .57868 .16650 .05000 1.00000 Uiso
H12a .59406 .46569 .12691 .05000 1.00000 Uiso
H13a .72034 .45156 .22865 .05000 1.00000 Uiso
H11b .58473 .70164 .00490 .05000 1.00000 Uiso
H12b .40204 .68339 -.06207 .05000 1.00000 Uiso
H13b .41828 .65101 .05428 .05000 1.00000 Uiso
H01 .356(12) .470(8) .244(7) .05000 1.00000 Uiso
H02 -.046(11) .347(8) .318(7) .05000 1.00000 Uiso
H03 -.166(11) .603(9) .549(7) .05000 1.00000 Uiso
H04 .131(12) .473(9) .736(7) .05000 1.00000 Uiso
H05 .476(10) .383(8) .722(6) .05000 1.00000 Uiso
H06 .704(11) .350(8) .492(7) .05000 1.00000 Uiso
H1a .590(11) .590(9) .291(7) .05000 1.00000 Uiso
H1b .511(11) .860(8) .075(6) .05000 1.00000 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 .021(5) .041(6) .031(5) -.003(4) .003(4) -.001(5)
N2 .021(5) .052(7) .021(5) .003(5) .006(4) .003(5)
N3 .022(5) .031(6) .028(5) .003(4) .004(4) .001(5)
N4 .032(5) .035(6) .021(5) .008(4) .005(4) .002(4)
N5 .025(5) .041(6) .023(5) .006(4) .001(4) .002(4)
N6 .026(5) .034(5) .021(5) .002(4) .005(4) -.004(5)
C1 .023(6) .030(6) .021(6) .002(5) .008(5) .001(5)
C2 .022(6) .036(7) .022(6) -.001(5) .006(4) -.008(5)
C3 .026(6) .036(7) .021(5) .003(5) .004(5) -.002(5)
C4 .022(5) .038(6) .021(5) -.000(5) -.000(4) -.005(5)
C5 .022(6) .039(7) .028(6) -.003(5) .004(5) -.004(5)
C6 .027(5) .034(6) .019(5) .008(5) .003(4) .001(5)
C7 .023(6) .041(7) .021(6) .000(5) .002(5) -.002(5)
C8 .027(6) .043(7) .028(6) -.001(6) .009(5) .008(6)
C9 .040(7) .061(8) .029(6) -.003(6) .007(5) .001(6)
C10 .046(7) .080(10) .029(6) .016(7) .005(6) .005(7)
C11 .033(7) .097(10) .034(7) -.012(7) -.001(5) -.012(8)
C12 .033(6) .078(9) .024(6) -.008(7) .006(5) -.007(7)
C13 .027(6) .047(7) .022(6) .004(5) .001(5) -.005(5)
C14 .029(6) .025(6) .027(6) -.000(5) .004(5) -.003(5)
C15 .026(6) .034(7) .026(6) .000(5) .012(5) -.001(5)
C16 .036(6) .038(7) .037(7) .006(6) .013(5) .002(6)
C17 .039(6) .053(8) .040(7) -.001(6) .019(6) -.008(7)
C18 .045(7) .057(8) .027(6) .003(7) .015(6) -.005(6)
C19 .053(7) .038(7) .029(6) .003(6) .015(5) -.001(6)
C20 .024(6) .044(8) .029(6) -.002(5) .008(5) -.009(6)
C21 .022(6) .025(7) .031(6) -.003(5) .002(5) -.003(5)
C22 .021(6) .030(7) .036(6) -.003(5) .005(5) .005(6)
C23 .034(6) .034(7) .025(6) .004(5) -.001(5) .003(5)
C24 .039(7) .045(8) .034(7) .005(6) -.001(6) .004(6)
C25 .024(6) .044(7) .040(7) .005(5) .003(5) -.002(6)
C26 .020(6) .034(7) .031(6) -.003(5) .002(5) -.004(5)
C27 .024(6) .031(6) .022(6) -.004(5) -.002(4) -.001(6)
O1a .035(5) .063(6) .046(5) -.010(4) .007(4) -.008(5)
C1a .043(8) .088(11) .051(8) .001(7) .006(6) -.002(8)
O1b .055(6) .113(9) .060(6) .012(6) -.010(5) -.009(6)
C1b .054(9) .123(14) .072(10) .009(9) .013(8) -.034(11)
Cl1 .0339(14) .0430(16) .0289(14) .0004(13) .0098(11) -.0015(13)
Cl2 .0392(15) .0417(16) .0282(14) .0002(14) .0025(11) -.0000(13)
Cl3 .0376(15) .094(3) .0312(15) .0082(16) .0090(12) .0156(16)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
N1 C7 . . 1.327(12)
N1 C8 . . 1.394(12)
N1 H01 . . .92(10)
N2 C7 . . 1.328(12)
N2 C13 . . 1.405(12)
N2 H02 . . .99(10)
N3 C14 . . 1.328(12)
N3 C15 . . 1.405(13)
N3 H03 . . .85(10)
N4 C14 . . 1.348(12)
N4 C20 . . 1.392(13)
N4 H04 . . .93(10)
N5 C21 . . 1.354(12)
N5 C22 . . 1.388(12)
N5 H05 . . 1.12(10)
N6 C21 . . 1.335(12)
N6 C27 . . 1.406(11)
N6 H06 . . .99(10)
C1 C2 . . 1.549(14)
C1 C6 . . 1.536(13)
C1 C7 . . 1.495(13)
C2 C3 . . 1.551(13)
C3 C4 . . 1.533(13)
C3 C14 . . 1.496(13)
C4 C5 . . 1.531(14)
C5 C6 . . 1.551(12)
C5 C21 . . 1.491(12)
C8 C9 . . 1.379(14)
C8 C13 . . 1.399(13)
C9 C10 . . 1.382(14)
C10 C11 . . 1.394(15)
C11 C12 . . 1.386(14)
C12 C13 . . 1.372(13)
C15 C16 . . 1.373(13)
C15 C20 . . 1.367(13)
C16 C17 . . 1.388(15)
C17 C18 . . 1.406(14)
C18 C19 . . 1.368(15)
C19 C20 . . 1.406(14)
C22 C23 . . 1.392(13)
C22 C27 . . 1.394(13)
C23 C24 . . 1.383(14)
C24 C25 . . 1.416(15)
C25 C26 . . 1.382(13)
C26 C27 . . 1.376(13)
O1a C1a . . 1.431(14)
O1a H1a . . 1.01(9)
O1b C1b . . 1.38(2)
O1b H1b . . 1.18(9)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
C7 N1 C8 . . . 109.8(8)
C7 N1 H01 . . . 125(7)
C8 N1 H01 . . . 125(7)
C7 N2 C13 . . . 109.0(8)
C7 N2 H02 . . . 129(6)
C13 N2 H02 . . . 122(6)
C14 N3 C15 . . . 109.4(8)
C14 N3 H03 . . . 133(7)
C15 N3 H03 . . . 118(7)
C14 N4 C20 . . . 108.2(8)
C14 N4 H04 . . . 125(7)
C20 N4 H04 . . . 127(7)
C21 N5 C22 . . . 108.3(8)
C21 N5 H05 . . . 119(5)
C22 N5 H05 . . . 132(5)
C21 N6 C27 . . . 109.7(8)
C21 N6 H06 . . . 125(6)
C27 N6 H06 . . . 125(6)
C2 C1 C6 . . . 110.9(8)
C2 C1 C7 . . . 111.8(8)
C6 C1 C7 . . . 110.5(8)
C1 C2 C3 . . . 107.1(7)
C2 C3 C4 . . . 111.4(8)
C2 C3 C14 . . . 113.3(8)
C4 C3 C14 . . . 109.7(8)
C3 C4 C5 . . . 111.3(8)
C4 C5 C6 . . . 111.8(7)
C4 C5 C21 . . . 108.4(8)
C6 C5 C21 . . . 112.5(8)
C1 C6 C5 . . . 108.6(8)
N1 C7 N2 . . . 109.4(8)
N1 C7 C1 . . . 123.9(8)
N2 C7 C1 . . . 126.7(8)
N1 C8 C9 . . . 132.0(9)
N1 C8 C13 . . . 105.8(8)
C9 C8 C13 . . . 122.2(9)
C8 C9 C10 . . . 115.5(10)
C9 C10 C11 . . . 122.5(10)
C10 C11 C12 . . . 121.6(10)
C11 C12 C13 . . . 116.1(9)
N2 C13 C8 . . . 106.1(8)
N2 C13 C12 . . . 131.8(9)
C8 C13 C12 . . . 122.1(9)
N3 C14 N4 . . . 108.8(9)
N3 C14 C3 . . . 126.4(8)
N4 C14 C3 . . . 124.5(8)
N3 C15 C16 . . . 131.5(9)
N3 C15 C20 . . . 105.9(8)
C16 C15 C20 . . . 122.6(9)
C15 C16 C17 . . . 116.5(9)
C16 C17 C18 . . . 121.1(10)
C17 C18 C19 . . . 122.0(10)
C18 C19 C20 . . . 116.0(9)
N4 C20 C15 . . . 107.8(8)
N4 C20 C19 . . . 130.4(9)
C15 C20 C19 . . . 121.8(9)
N5 C21 N6 . . . 108.9(8)
N5 C21 C5 . . . 125.6(8)
N6 C21 C5 . . . 125.3(8)
N5 C22 C23 . . . 130.7(9)
N5 C22 C27 . . . 107.9(8)
C23 C22 C27 . . . 121.4(9)
C22 C23 C24 . . . 116.2(9)
C23 C24 C25 . . . 122.5(9)
C24 C25 C26 . . . 120.2(9)
C25 C26 C27 . . . 117.6(9)
N6 C27 C22 . . . 105.1(8)
N6 C27 C26 . . . 132.7(8)
C22 C27 C26 . . . 122.2(8)
C1a O1a H1a . . . 102(6)
C1b O1b H1b . . . 111(5)

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
C8 N1 C7 N2 . . . . .9(12)
C8 N1 C7 C1 . . . . -179.5(9)
H01 N1 C7 N2 . . . . 178(8)
H01 N1 C7 C1 . . . . -2(8)
C7 N1 C8 C9 . . . . 177.8(12)
C7 N1 C8 C13 . . . . -.8(12)
H01 N1 C8 C9 . . . . 0(8)
H01 N1 C8 C13 . . . . -178(8)
C13 N2 C7 N1 . . . . -.6(11)
C13 N2 C7 C1 . . . . 179.8(10)
H02 N2 C7 N1 . . . . -178(7)
H02 N2 C7 C1 . . . . 2(7)
C7 N2 C13 C8 . . . . .1(11)
C7 N2 C13 C12 . . . . -178.5(12)
H02 N2 C13 C8 . . . . 178(7)
H02 N2 C13 C12 . . . . 0(7)
C15 N3 C14 N4 . . . . .4(11)
C15 N3 C14 C3 . . . . -174.1(9)
H03 N3 C14 N4 . . . . -180(8)
H03 N3 C14 C3 . . . . 6(9)
C14 N3 C15 C16 . . . . -179.3(11)
C14 N3 C15 C20 . . . . -1.1(11)
H03 N3 C15 C16 . . . . 1(8)
H03 N3 C15 C20 . . . . 179(8)
C20 N4 C14 N3 . . . . .4(11)
C20 N4 C14 C3 . . . . 175.1(9)
H04 N4 C14 N3 . . . . 176(8)
H04 N4 C14 C3 . . . . -9(8)
C14 N4 C20 C15 . . . . -1.1(11)
C14 N4 C20 C19 . . . . 178.4(11)
H04 N4 C20 C15 . . . . -177(8)
H04 N4 C20 C19 . . . . 3(8)
C22 N5 C21 N6 . . . . .9(11)
C22 N5 C21 C5 . . . . -174.6(9)
H05 N5 C21 N6 . . . . 170(6)
H05 N5 C21 C5 . . . . -5(6)
C21 N5 C22 C23 . . . . 179.0(11)
C21 N5 C22 C27 . . . . -.6(11)
H05 N5 C22 C23 . . . . 11(7)
H05 N5 C22 C27 . . . . -168(7)
C27 N6 C21 N5 . . . . -.9(11)
C27 N6 C21 C5 . . . . 174.6(9)
H06 N6 C21 N5 . . . . -176(7)
H06 N6 C21 C5 . . . . 0(7)
C21 N6 C27 C22 . . . . .6(11)
C21 N6 C27 C26 . . . . -177.3(11)
H06 N6 C27 C22 . . . . 175(7)
H06 N6 C27 C26 . . . . -3(7)
C6 C1 C2 C3 . . . . 62.3(10)
C7 C1 C2 C3 . . . . -173.8(8)
C2 C1 C6 C5 . . . . -61.1(10)
C7 C1 C6 C5 . . . . 174.3(8)
C2 C1 C7 N1 . . . . 164.9(9)
C2 C1 C7 N2 . . . . -15.6(14)
C6 C1 C7 N1 . . . . -71.0(12)
C6 C1 C7 N2 . . . . 108.5(11)
C1 C2 C3 C4 . . . . -58.9(10)
C1 C2 C3 C14 . . . . 176.9(8)
C2 C3 C4 C5 . . . . 56.0(11)
C14 C3 C4 C5 . . . . -177.8(8)
C2 C3 C14 N3 . . . . -50.0(13)
C2 C3 C14 N4 . . . . 136.3(10)
C4 C3 C14 N3 . . . . -175.2(9)
C4 C3 C14 N4 . . . . 11.1(13)
C3 C4 C5 C6 . . . . -54.0(11)
C3 C4 C5 C21 . . . . -178.6(8)
C4 C5 C6 C1 . . . . 56.0(10)
C21 C5 C6 C1 . . . . 178.3(8)
C4 C5 C21 N5 . . . . -12.0(13)
C4 C5 C21 N6 . . . . 173.1(9)
C6 C5 C21 N5 . . . . -136.1(9)
C6 C5 C21 N6 . . . . 49.0(12)
N1 C8 C9 C10 . . . . -178.9(11)
C13 C8 C9 C10 . . . . -.5(17)
N1 C8 C13 N2 . . . . .4(11)
N1 C8 C13 C12 . . . . 179.1(10)
C9 C8 C13 N2 . . . . -178.4(10)
C9 C8 C13 C12 . . . . .3(17)
C8 C9 C10 C11 . . . . 1.1(18)
C9 C10 C11 C12 . . . . -2(2)
C10 C11 C12 C13 . . . . 1.5(19)
C11 C12 C13 N2 . . . . 177.6(11)
C11 C12 C13 C8 . . . . -.8(17)
N3 C15 C16 C17 . . . . 177.5(11)
C20 C15 C16 C17 . . . . -.4(16)
N3 C15 C20 N4 . . . . 1.3(11)
N3 C15 C20 C19 . . . . -178.3(9)
C16 C15 C20 N4 . . . . 179.7(10)
C16 C15 C20 C19 . . . . .1(16)
C15 C16 C17 C18 . . . . -.2(16)
C16 C17 C18 C19 . . . . 1.1(18)
C17 C18 C19 C20 . . . . -1.4(16)
C18 C19 C20 N4 . . . . -178.7(11)
C18 C19 C20 C15 . . . . .8(15)
N5 C22 C23 C24 . . . . -178.5(10)
C27 C22 C23 C24 . . . . 1.0(15)
N5 C22 C27 N6 . . . . -.0(11)
N5 C22 C27 C26 . . . . 178.2(9)
C23 C22 C27 N6 . . . . -179.6(9)
C23 C22 C27 C26 . . . . -1.4(16)
C22 C23 C24 C25 . . . . -.2(15)
C23 C24 C25 C26 . . . . -.1(16)
C24 C25 C26 C27 . . . . -.3(15)
C25 C26 C27 N6 . . . . 178.7(11)
C25 C26 C27 C22 . . . . 1.0(15)

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H01 O1a . . . 0.92(10) 1.77(10) 2.681(10) 172(9)
N2 H02 Cl1 . . 2_546 0.99(9) 2.10(9) 3.062(8) 165(7)
N3 H03 Cl2 . . 2_556 0.85(9) 2.20(9) 3.034(8) 166(9)
N4 H04 Cl3 . . . 0.93(9) 2.22(9) 3.144(8) 171(9)
N5 H05 Cl3 . . . 1.12(9) 2.09(9) 3.163(8) 159(7)
N6 H06 Cl1 . . 2_646 0.99(10) 2.19(10) 3.075(8) 149(7)
O1a H1a Cl2 . . 2_656 1.01(9) 2.12(9) 3.085(7) 160(8)
O1b H1b Cl3 . . 2_656 1.18(8) 1.97(8) 3.127(8) 166(7)

#=END==============================================================

# Attachment '5bH3.cif'

data_5bH3
_database_code_depnum_ccdc_archive 'CCDC 602154'

#--(C30H33Br3N6)(H2O)4 ---------------------------------- [5bH3]Br3.4H2O ---

_audit_creation_date             2005-10-10
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2005-12-05
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1

_chemical_formula_moiety         'C30 H33 N6 , Br3 , (H2 O)4'
_chemical_formula_sum            'C30 H41 Br3 N6 O4'
_chemical_formula_weight         789.5

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-y,+x-y,+z
-x+y,-x,+z
-x,-y,-z
+y,-x+y,-z
+x-y,+x,-z
2/3+x,1/3+y,1/3+z
1/3+x,2/3+y,2/3+z
2/3-y,1/3+x-y,1/3+z
1/3-y,2/3+x-y,2/3+z
2/3-x+y,1/3-x,1/3+z
1/3-x+y,2/3-x,2/3+z
2/3-x,1/3-y,1/3-z
1/3-x,2/3-y,2/3-z
2/3+y,1/3-x+y,1/3-z
1/3+y,2/3-x+y,2/3-z
2/3+x-y,1/3+x,1/3-z
1/3+x-y,2/3+x,2/3-z
_cell_length_a                   16.6939(9)
_cell_length_b                   16.6939(9)
_cell_length_c                   20.5208(11)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                120.0000
_cell_volume                     4952.7(5)
_cell_formula_units_Z            6
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      not_measured
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_cell_measurement_reflns_used    7998
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      28.0
_cell_measurement_temperature    200
_exptl_crystal_F_000             2400
_exptl_absorpt_coefficient_mu    3.71
_exptl_crystal_description       prism
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .19
_exptl_crystal_size_min          .11
_exptl_crystal_colour            yellow

_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_detector_area_resol_mean 6
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED; Stoe & Cie, 1999'
_exptl_absorpt_correction_T_min  .504
_exptl_absorpt_correction_T_max  .6807
_diffrn_reflns_number            22725
_reflns_number_total             2665
_reflns_number_gt                1505
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_diffrn_reflns_theta_max         28.0
_diffrn_reflns_theta_full        28.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measured_fraction_theta_full 1.0
_diffrn_reflns_av_R_equivalents  .087
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_standards_decay_%        0

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .028
_refine_ls_wR_factor_ref         .028
_refine_ls_goodness_of_fit_ref   1.12(2)
_refine_ls_number_reflns         1598
_refine_ls_number_parameters     140
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.0002(Fo^2^)]
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          .006
_refine_diff_density_max         .783
_refine_diff_density_min         -.849
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .00000
_refine_ls_abs_structure_details none

_refine_special_details          
;
Hydrogen treatment:
- Hydrogen of H2O were observed and refined with restraints on bond
lengths and bond angles (fixed Uiso).
- Other H atoms: calculated.
;

_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_structure_solution    SIR97
_computing_structure_refinement  xtal_CRYLSQ
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO

loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
Br Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 -.374 2.456
N Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .004 .003
O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006

loop_
_atom_site_label
_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
Br .42285(3) .35551(3) .411871(18) .04030(18) 1.00000 Uani
N1 .84073(14) .56796(14) .57738(11) .0179(10) 1.00000 Uani
N2 .76013(15) .59912(14) .50850(11) .0193(10) 1.00000 Uani
C1 .87069(17) .66188(17) .58395(14) .0181(12) 1.00000 Uani
C2 .93728(18) .73000(18) .62435(14) .0221(12) 1.00000 Uani
C3 .94899(19) .81770(19) .61822(14) .0265(13) 1.00000 Uani
C4 .8961(2) .83688(18) .57454(15) .0272(14) 1.00000 Uani
C5 .82960(18) .76942(18) .53505(15) .0248(13) 1.00000 Uani
C6 .81856(17) .68102(17) .54030(14) .0186(12) 1.00000 Uani
C7 .77491(16) .53240(17) .53180(13) .0172(11) 1.00000 Uani
C8 .72209(17) .43390(17) .51103(13) .0188(12) 1.00000 Uani
C9 .76760(17) .37914(17) .53521(14) .0191(12) 1.00000 Uani
C10 .6995(2) .59033(19) .45353(15) .0295(14) 1.00000 Uani
O1w .49073(16) .43106(15) .64816(12) .0387(11) 1.00000 Uani
O2w .7012(14) .2578(12) .3174(8) .133(5) .33333 Uiso
H01 .86414 .53353 .60210 .04000 1.00000 Uiso
H2 .97364 .71632 .65530 .04000 1.00000 Uiso
H3 .99630 .86817 .64489 .04000 1.00000 Uiso
H4 .90614 .89988 .57233 .04000 1.00000 Uiso
H5 .79259 .78292 .50471 .04000 1.00000 Uiso
H8 .72188 .43234 .46315 .04000 1.00000 Uiso
H91 .83097 .40756 .51862 .04000 1.00000 Uiso
H92 .76871 .37962 .58305 .04000 1.00000 Uiso
H101 .65194 .60184 .46836 .04000 1.00000 Uiso
H102 .73563 .63488 .42039 .04000 1.00000 Uiso
H103 .67238 .52947 .43559 .04000 1.00000 Uiso
H11w .4465(18) .4243(18) .6757(14) .04000 1.00000 Uiso
H12w .5104(19) .4834(16) .6252(14) .04000 1.00000 Uiso
H02w .7364(15) .308(3) .343(3) .04000 .66667 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Br .0425(3) .0406(2) .0373(2) .02037(17) -.00809(16) .00568(17)
N1 .0160(11) .0158(11) .0213(12) .0075(9) .0017(9) .0025(9)
N2 .0172(11) .0161(11) .0250(13) .0086(9) -.0021(10) .0021(10)
C1 .0160(12) .0177(13) .0222(15) .0096(11) .0060(11) .0031(11)
C2 .0185(13) .0236(14) .0212(15) .0084(12) .0028(12) .0017(12)
C3 .0212(14) .0223(14) .0278(18) .0047(12) .0036(12) -.0060(13)
C4 .0294(15) .0166(14) .0356(19) .0115(12) .0082(13) .0016(12)
C5 .0238(14) .0184(14) .0341(18) .0118(12) .0019(13) .0025(12)
C6 .0145(13) .0167(13) .0232(16) .0068(11) .0038(11) .0017(11)
C7 .0149(13) .0185(13) .0194(15) .0093(11) .0032(11) .0035(11)
C8 .0169(13) .0164(13) .0217(15) .0073(11) .0006(11) .0009(11)
C9 .0146(13) .0154(13) .0273(16) .0076(11) -.0007(11) .0008(11)
C10 .0328(16) .0243(15) .0340(18) .0162(13) -.0116(14) .0008(13)
O1w .0406(14) .0270(11) .0426(15) .0124(11) .0031(11) -.0071(10)

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
N1 C1 . . 1.394(4)
N1 C7 . . 1.335(4)
N2 C6 . . 1.383(3)
N2 C7 . . 1.343(5)
N2 C10 . . 1.473(4)
C1 C2 . . 1.397(4)
C1 C6 . . 1.393(5)
C2 C3 . . 1.382(5)
C3 C4 . . 1.403(5)
C4 C5 . . 1.381(4)
C5 C6 . . 1.397(5)
C7 C8 . . 1.488(4)
C8 C9 . . 1.534(5)
C8 C9 . 2_655 1.548(4)
O1w H11w . . .89(4)
O1w H12w . . .90(3)
O2w H02w . . .91(4)
O2w H02w . 16 .89(5)

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
C1 N1 C7 . . . 108.7(3)
C6 N2 C7 . . . 108.7(3)
C6 N2 C10 . . . 124.7(3)
C7 N2 C10 . . . 126.3(3)
N1 C1 C2 . . . 131.7(3)
N1 C1 C6 . . . 106.4(3)
C2 C1 C6 . . . 121.9(3)
C1 C2 C3 . . . 116.2(3)
C2 C3 C4 . . . 121.9(3)
C3 C4 C5 . . . 122.0(3)
C4 C5 C6 . . . 116.4(3)
N2 C6 C1 . . . 106.8(3)
N2 C6 C5 . . . 131.5(3)
C1 C6 C5 . . . 121.6(3)
N1 C7 N2 . . . 109.4(3)
N1 C7 C8 . . . 126.4(3)
N2 C7 C8 . . . 124.1(3)
C7 C8 C9 . . . 111.7(3)
C7 C8 C9 . . 2_655 110.4(3)
C9 C8 C9 . . 2_655 110.4(3)
C8 C9 C8 . . 3_665 109.9(3)
H11w O1w H12w . . . 109(3)
H02w O2w H02w . . 16 110(5)
O2w H02w O2w . . 18_545 154(6)

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
C7 N1 C1 C2 . . . . 179.9(3)
C7 N1 C1 C6 . . . . .7(3)
C1 N1 C7 N2 . . . . -.4(3)
C1 N1 C7 C8 . . . . -177.9(3)
C7 N2 C6 C1 . . . . .5(3)
C7 N2 C6 C5 . . . . -178.8(3)
C10 N2 C6 C1 . . . . -173.6(3)
C10 N2 C6 C5 . . . . 7.1(5)
C6 N2 C7 N1 . . . . -.1(3)
C6 N2 C7 C8 . . . . 177.5(3)
C10 N2 C7 N1 . . . . 173.9(3)
C10 N2 C7 C8 . . . . -8.5(5)
N1 C1 C2 C3 . . . . -179.6(3)
C6 C1 C2 C3 . . . . -.4(5)
N1 C1 C6 N2 . . . . -.7(3)
N1 C1 C6 C5 . . . . 178.7(3)
C2 C1 C6 N2 . . . . 180.0(3)
C2 C1 C6 C5 . . . . -.6(5)
C1 C2 C3 C4 . . . . .9(5)
C2 C3 C4 C5 . . . . -.3(5)
C3 C4 C5 C6 . . . . -.8(5)
C4 C5 C6 N2 . . . . -179.6(3)
C4 C5 C6 C1 . . . . 1.2(5)
N1 C7 C8 C9 . . . . -14.6(4)
N1 C7 C8 C9 . . . 2_655 108.6(4)
N2 C7 C8 C9 . . . . 168.2(3)
N2 C7 C8 C9 . . . 2_655 -68.6(4)
C7 C8 C9 C8 . . . 3_665 -178.6(3)
C9 C8 C9 C8 2_655 . . 3_665 58.2(4)
H02w O2w H02w O2w 16 . . 18_545 -112(13)

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA

O1w H11w Br . . 9_555 0.89(3) 2.53(3) 3.419(3) 175(2)
O1w H12w Br . . 4_666 0.90(3) 2.46(2) 3.340(2) 166(2)
N1 H01 O1w . . 3_665 0.98 1.79 2.732(5) 161

#=END======================================================================