#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:15:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179101 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/63/4306367.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306367
loop_
_publ_author_name
'Patrick L. Feng'
'Changhyun Koo'
'John J. Henderson'
'Motohiro Nakano'
'Stephen Hill'
'Enrique del Barco'
'David N. Hendrickson'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of California-San Diego
La Jolla, CA 92093
USA
;
_publ_contact_author_email       dhendrickson@ucsd.edu
_publ_contact_author_name        'David N. Hendrickson'
_publ_section_title
;
Single-Molecule-Magnet Behavior and Spin Changes Affected by Crystal
Packing Effects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8610
_journal_page_last               8612
_journal_paper_doi               10.1021/ic801208z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C21 H12 Br2 Mn3 N21 O7 Zn2, 3(C8 H20 N)'
_chemical_formula_sum            'C45 H72 Br2 Mn3 N24 O7 Zn2'
_chemical_formula_weight         1516.67
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.4023(17)
_cell_length_b                   13.4023(17)
_cell_length_c                   60.923(8)
_cell_measurement_reflns_used    3118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.21
_cell_volume                     9477(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            21402
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    2.666
_exptl_absorpt_correction_T_max  0.593
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             4650
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0182P)²+6.8033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                3391
_reflns_number_total             3551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801208z_si_002_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4306367
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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
O3 O 0.00347(16) 0.79643(14) 0.89183(3) 0.0178(4) Uani 1 1 d . . .
N8 N 0.38444(19) 0.40144(19) 0.84054(4) 0.0214(5) Uani 1 1 d . . .
C12 C 0.3256(2) 0.4304(2) 0.85870(4) 0.0241(6) Uani 1 1 d . . .
H12A H 0.2582 0.4293 0.8526 0.029 Uiso 1 1 calc R . .
H12B H 0.2989 0.3703 0.8697 0.029 Uiso 1 1 calc R . .
C4 C -0.5260(2) 0.5368(2) 0.93197(5) 0.0257(7) Uani 1 1 d . . .
H4 H -0.5919 0.5018 0.9406 0.031 Uiso 1 1 calc R . .
C9 C 0.3388(3) 0.2356(3) 0.81396(5) 0.0340(7) Uani 1 1 d . . .
H9A H 0.3609 0.2860 0.8015 0.051 Uiso 1 1 calc R . .
H9B H 0.2781 0.1603 0.8098 0.051 Uiso 1 1 calc R . .
H9C H 0.4039 0.2305 0.8190 0.051 Uiso 1 1 calc R . .
C11 C 0.4703(3) 0.3139(3) 0.86636(5) 0.0302(7) Uani 1 1 d . . .
H11A H 0.4278 0.3211 0.8783 0.045 Uiso 1 1 calc R . .
H11B H 0.5427 0.3252 0.8716 0.045 Uiso 1 1 calc R . .
H11C H 0.4269 0.2385 0.8600 0.045 Uiso 1 1 calc R . .
C14 C 0.4243(3) 0.4897(3) 0.82224(5) 0.0307(7) Uani 1 1 d . . .
H14A H 0.4815 0.5638 0.8281 0.037 Uiso 1 1 calc R . .
H14B H 0.4620 0.4683 0.8111 0.037 Uiso 1 1 calc R . .
C3 C -0.4763(2) 0.4734(2) 0.92425(5) 0.0283(7) Uani 1 1 d . . .
H3 H -0.5102 0.3954 0.9276 0.034 Uiso 1 1 calc R . .
C13 C 0.3987(3) 0.5448(3) 0.86986(5) 0.0304(7) Uani 1 1 d . . .
H13A H 0.4651 0.5469 0.8762 0.046 Uiso 1 1 calc R . .
H13B H 0.3545 0.5549 0.8812 0.046 Uiso 1 1 calc R . .
H13C H 0.4229 0.6057 0.8593 0.046 Uiso 1 1 calc R . .
C8 C 0.2967(2) 0.2826(2) 0.83217(5) 0.0261(6) Uani 1 1 d . . .
H8A H 0.2719 0.2292 0.8444 0.031 Uiso 1 1 calc R . .
H8B H 0.2299 0.2854 0.8269 0.031 Uiso 1 1 calc R . .
C10 C 0.4917(2) 0.4036(3) 0.84917(5) 0.0269(7) Uani 1 1 d . . .
H10A H 0.5316 0.3930 0.8369 0.032 Uiso 1 1 calc R . .
H10B H 0.5424 0.4791 0.8553 0.032 Uiso 1 1 calc R . .
C15 C 0.3309(3) 0.5033(3) 0.81141(6) 0.0465(9) Uani 1 1 d . . .
H15A H 0.2720 0.4299 0.8060 0.070 Uiso 1 1 calc R . .
H15B H 0.3630 0.5563 0.7994 0.070 Uiso 1 1 calc R . .
H15C H 0.2983 0.5323 0.8219 0.070 Uiso 1 1 calc R . .
Zn2 Zn 0.0000 1.0000 0.843733(8) 0.01478(13) Uani 1 3 d S . .
Br1 Br 0.0000 1.0000 0.982312(7) 0.02317(13) Uani 1 3 d S . .
Zn1 Zn 0.0000 1.0000 0.943444(8) 0.01543(13) Uani 1 3 d S . .
Br2 Br 0.0000 1.0000 0.804979(7) 0.02246(13) Uani 1 3 d S . .
Mn5 Mn -0.11220(3) 0.84169(3) 0.894093(8) 0.01467(9) Uani 1 1 d . . .
N4 N -0.12907(19) 0.85425(19) 0.85663(3) 0.0173(5) Uani 1 1 d . . .
O1 O 0.0000 1.0000 0.89368(7) 0.0137(6) Uani 1 3 d S . .
N1 N -0.0929(2) 0.83953(19) 0.93167(4) 0.0183(5) Uani 1 1 d . . .
N5 N -0.2219(2) 0.79068(19) 0.84854(3) 0.0193(5) Uani 1 1 d . . .
O2 O -0.23057(14) 0.68788(14) 0.89380(3) 0.0193(4) Uani 1 1 d . . .
N7 N 0.11117(18) 0.87982(18) 0.89852(3) 0.0174(5) Uani 1 1 d . . .
N3 N -0.0670(3) 0.6906(3) 0.94604(4) 0.0462(8) Uani 1 1 d . . .
N2 N -0.0787(2) 0.7649(2) 0.93923(4) 0.0231(5) Uani 1 1 d . . .
C6 C -0.3753(2) 0.7070(2) 0.91362(4) 0.0181(5) Uani 1 1 d . . .
C5 C -0.4761(2) 0.6517(2) 0.92659(4) 0.0228(6) Uani 1 1 d . . .
H5 H -0.5095 0.6939 0.9316 0.027 Uiso 1 1 calc R . .
C1 C -0.3242(2) 0.6428(2) 0.90638(4) 0.0181(5) Uani 1 1 d . . .
N6 N -0.3116(2) 0.7264(2) 0.84144(4) 0.0309(6) Uani 1 1 d . . .
C2 C -0.3769(2) 0.5257(2) 0.91169(5) 0.0237(6) Uani 1 1 d . . .
H2 H -0.3447 0.4824 0.9067 0.028 Uiso 1 1 calc R . .
C7 C 0.1738(2) 0.8424(2) 0.90772(5) 0.0182(6) Uani 1 1 d . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
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
N7 O3 Mn5 113.91(14) . . ?
C14 N8 C12 111.3(2) . . ?
C14 N8 C10 106.2(2) . . ?
C12 N8 C10 110.6(2) . . ?
C14 N8 C8 110.9(2) . . ?
C12 N8 C8 106.5(2) . . ?
C10 N8 C8 111.4(2) . . ?
C13 C12 N8 115.6(2) . . ?
C5 C4 C3 119.2(3) . . ?
C15 C14 N8 115.3(3) . . ?
C2 C3 C4 120.5(3) . . ?
C9 C8 N8 115.4(2) . . ?
C11 C10 N8 115.1(2) . . ?
N4 Zn2 N4 105.73(7) 2_675 . ?
N4 Zn2 N4 105.73(7) 2_675 3_465 ?
N4 Zn2 N4 105.73(7) . 3_465 ?
N4 Zn2 Br2 113.00(6) 2_675 . ?
N4 Zn2 Br2 113.00(6) . . ?
N4 Zn2 Br2 113.00(6) 3_465 . ?
N1 Zn1 N1 107.91(7) . 2_675 ?
N1 Zn1 N1 107.91(7) . 3_465 ?
N1 Zn1 N1 107.91(7) 2_675 3_465 ?
N1 Zn1 Br1 110.99(7) . . ?
N1 Zn1 Br1 110.99(7) 2_675 . ?
N1 Zn1 Br1 110.99(7) 3_465 . ?
O2 Mn5 O1 176.03(7) . . ?
O2 Mn5 O3 91.42(7) . . ?
O1 Mn5 O3 92.21(6) . . ?
O2 Mn5 N7 88.76(8) . 3_465 ?
O1 Mn5 N7 87.71(7) . 3_465 ?
O3 Mn5 N7 176.36(8) . 3_465 ?
O2 Mn5 N1 91.96(8) . . ?
O1 Mn5 N1 89.78(13) . . ?
O3 Mn5 N1 87.38(8) . . ?
N7 Mn5 N1 88.98(8) 3_465 . ?
O2 Mn5 N4 90.62(8) . . ?
O1 Mn5 N4 87.52(13) . . ?
O3 Mn5 N4 94.34(8) . . ?
N7 Mn5 N4 89.29(9) 3_465 . ?
N1 Mn5 N4 176.85(8) . . ?
N5 N4 Zn2 127.46(18) . . ?
N5 N4 Mn5 117.17(17) . . ?
Zn2 N4 Mn5 112.90(10) . . ?
Mn5 O1 Mn5 119.982(7) 2_675 . ?
Mn5 O1 Mn5 119.982(7) 2_675 3_465 ?
Mn5 O1 Mn5 119.982(7) . 3_465 ?
N2 N1 Zn1 119.0(2) . . ?
N2 N1 Mn5 117.22(18) . . ?
Zn1 N1 Mn5 110.83(10) . . ?
N6 N5 N4 177.2(3) . . ?
C1 O2 Mn5 125.65(15) . . ?
C7 N7 O3 115.6(2) . . ?
C7 N7 Mn5 125.49(18) . 2_675 ?
O3 N7 Mn5 118.88(15) . 2_675 ?
N3 N2 N1 177.9(3) . . ?
C1 C6 C5 118.9(2) . . ?
C1 C6 C7 122.9(2) . 3_465 ?
C5 C6 C7 118.2(2) . 3_465 ?
C4 C5 C6 121.4(3) . . ?
O2 C1 C2 118.3(2) . . ?
O2 C1 C6 122.6(2) . . ?
C2 C1 C6 119.0(2) . . ?
C3 C2 C1 120.9(3) . . ?
N7 C7 C6 122.6(2) . 2_675 ?
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
O3 N7 1.373(3) . ?
O3 Mn5 1.9314(18) . ?
N8 C14 1.515(3) . ?
N8 C12 1.518(3) . ?
N8 C10 1.517(4) . ?
N8 C8 1.519(3) . ?
C12 C13 1.507(4) . ?
C4 C5 1.377(4) . ?
C4 C3 1.398(5) . ?
C9 C8 1.517(4) . ?
C11 C10 1.509(4) . ?
C14 C15 1.505(5) . ?
C3 C2 1.385(4) . ?
Zn2 N4 2.012(2) 2_675 ?
Zn2 N4 2.012(2) . ?
Zn2 N4 2.012(2) 3_465 ?
Zn2 Br2 2.3610(7) . ?
Br1 Zn1 2.3680(7) . ?
Zn1 N1 2.003(2) . ?
Zn1 N1 2.003(2) 2_675 ?
Zn1 N1 2.003(2) 3_465 ?
Mn5 O2 1.8698(18) . ?
Mn5 O1 1.8903(5) . ?
Mn5 N7 2.008(2) 3_465 ?
Mn5 N1 2.305(2) . ?
Mn5 N4 2.308(2) . ?
N4 N5 1.207(3) . ?
O1 Mn5 1.8903(5) 2_675 ?
O1 Mn5 1.8903(5) 3_465 ?
N1 N2 1.199(3) . ?
N5 N6 1.157(3) . ?
O2 C1 1.330(3) . ?
N7 C7 1.301(4) . ?
N7 Mn5 2.008(2) 2_675 ?
N3 N2 1.160(3) . ?
C6 C1 1.412(4) . ?
C6 C5 1.414(4) . ?
C6 C7 1.445(4) 3_465 ?
C1 C2 1.400(4) . ?
C7 C6 1.445(4) 2_675 ?
