#------------------------------------------------------------------------------
#$Date: 2015-07-05 11:41:33 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140103 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/37/4123758.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_4123758
loop_
_publ_author_name
'Nguyen, Tu N.'
'Shiddiq, Muhandis'
'Ghosh, Tuhin'
'Abboud, Khalil A.'
'Hill, Stephen'
'Christou, George'
_publ_section_title
;
 Covalently Linked Dimer of Mn3 Single-Molecule Magnets and Retention of
 Its Structure and Quantum Properties in Solution.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7160
_journal_page_last               7168
_journal_paper_doi               10.1021/jacs.5b02677
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C51 H48 I6 Mn6 N12 O20'
_chemical_formula_weight         2240.05
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2013-11-22 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.5692(10)
_cell_length_b                   16.5692(10)
_cell_length_c                   18.2847(11)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     4347.3(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.419
_exptl_absorpt_coefficient_mu    3.036
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_meas      0
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.067
_platon_squeeze_details
;
;
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0697P)²+5.3861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2818
_reflns_number_total             3349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b02677_si_002.cif
_cod_data_source_block           tu88
_cod_depositor_comments          'Adding full bibliography for 4123758.cif.'
_cod_original_cell_volume        4347.3(6)
_cod_database_code               4123758
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.822
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_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, -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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.24618(3) -0.29481(3) 0.41669(2) 0.02713(15) Uani 1 1 d . . .
O1 O 0.19670(13) -0.46514(13) 0.33542(10) 0.0281(4) Uani 1 1 d . . .
O2 O 0.29176(15) -0.19875(15) 0.49092(12) 0.0380(5) Uani 1 1 d . . .
O3 O 0.3333 -0.3333 0.43253(17) 0.0278(7) Uani 1 3 d S T P
O4 O 0.15330(15) -0.40222(15) 0.49486(12) 0.0374(5) Uani 1 1 d . . .
N1 N 0.15005(17) -0.26380(17) 0.37743(13) 0.0311(5) Uani 1 1 d . . .
N2 N 0.17936(16) -0.39628(15) 0.34219(12) 0.0253(4) Uani 1 1 d . . .
C1 C 0.11608(18) -0.39357(18) 0.30269(14) 0.0266(5) Uani 1 1 d . . .
C2 C 0.0585(3) -0.47077(13) 0.2500 0.0296(8) Uani 1 2 d S T P
H2A H 0.0191 -0.4546 0.2232 0.036 Uiso 0.5 1 d R U P
C4 C 0.10157(19) -0.3154(2) 0.31922(15) 0.0302(6) Uani 1 1 d . . .
C7 C 0.3757(2) -0.1487(2) 0.51577(16) 0.0384(7) Uani 1 1 d . . .
C9 C 0.0433(2) -0.2932(2) 0.28049(19) 0.0419(7) Uani 1 1 d . . .
H9A H 0.0098 -0.3290 0.2391 0.050 Uiso 1 1 calc R U .
C10 C 0.1408(2) -0.1910(2) 0.3991(2) 0.0436(7) Uani 1 1 d . . .
H10A H 0.1753 -0.1554 0.4403 0.052 Uiso 1 1 calc R U .
C11 C 0.0347(3) -0.2181(3) 0.3031(2) 0.0554(10) Uani 1 1 d . . .
H11A H -0.0047 -0.2019 0.2770 0.066 Uiso 1 1 calc R U .
C13 C 0.0831(3) -0.1669(3) 0.3634(2) 0.0544(9) Uani 1 1 d . . .
H13A H 0.0766 -0.1160 0.3798 0.065 Uiso 1 1 calc R U .
C14 C 0.3871(3) -0.0807(3) 0.5749(2) 0.0604(11) Uani 1 1 d . . .
H14A H 0.4503 -0.0269 0.5730 0.091 Uiso 1 1 calc R U .
H14B H 0.3766 -0.1111 0.6227 0.091 Uiso 1 1 calc R U .
H14C H 0.3418 -0.0599 0.5675 0.091 Uiso 1 1 calc R U .
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'
I I -0.4742 1.8119 '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
O3 Mn1 O2 96.99(10) . .
O3 Mn1 N2 90.91(9) . .
O2 Mn1 N2 171.06(9) . .
O3 Mn1 N1 167.66(11) . .
O2 Mn1 N1 94.17(10) . .
N2 Mn1 N1 78.4(1) . .
O3 Mn1 O1 89.36(8) . 3_655
O2 Mn1 O1 91.44(8) . 3_655
N2 Mn1 O1 92.83(8) . 3_655
N1 Mn1 O1 85.08(8) . 3_655
O3 Mn1 O4 88.31(8) . .
O2 Mn1 O4 92.13(9) . .
N2 Mn1 O4 83.90(9) . .
N1 Mn1 O4 96.56(9) . .
O1 Mn1 O4 175.95(8) 3_655 .
O3 Mn1 Mn1 31.18(2) . 2_545
O2 Mn1 Mn1 122.59(7) . 2_545
N2 Mn1 Mn1 63.69(6) . 2_545
N1 Mn1 Mn1 140.96(7) . 2_545
O1 Mn1 Mn1 104.84(5) 3_655 2_545
O4 Mn1 Mn1 71.58(6) . 2_545
O3 Mn1 Mn1 31.18(2) . 3_655
O2 Mn1 Mn1 82.25(7) . 3_655
N2 Mn1 Mn1 106.69(6) . 3_655
N1 Mn1 Mn1 147.15(7) . 3_655
O1 Mn1 Mn1 62.49(5) 3_655 3_655
O4 Mn1 Mn1 116.15(6) . 3_655
Mn1 Mn1 Mn1 60.0 2_545 3_655
N2 O1 Mn1 112.28(15) . 2_545
C7 O2 Mn1 128.73(19) . .
Mn1 O3 Mn1 117.65(5) 2_545 3_655
Mn1 O3 Mn1 117.64(5) 2_545 .
Mn1 O3 Mn1 117.64(5) 3_655 .
C7 O4 Mn1 131.96(19) 2_545 .
C10 N1 C4 120.0(3) . .
C10 N1 Mn1 125.1(2) . .
C4 N1 Mn1 114.30(18) . .
C1 N2 O1 120.7(2) . .
C1 N2 Mn1 117.80(18) . .
O1 N2 Mn1 121.43(17) . .
N2 C1 C4 114.3(2) . .
N2 C1 C2 120.7(2) . .
C4 C1 C2 124.8(2) . .
C1 C2 C1 113.2(3) 6_545 .
C1 C2 H2A 109.2 6_545 .
C1 C2 H2A 108.8 . .
N1 C4 C9 120.5(3) . .
N1 C4 C1 114.5(2) . .
C9 C4 C1 125.0(3) . .
O4 C7 O2 125.4(3) 3_655 .
O4 C7 C14 119.5(3) 3_655 .
O2 C7 C14 115.1(3) . .
C11 C9 C4 118.9(3) . .
C11 C9 H9A 120.5 . .
C4 C9 H9A 120.5 . .
N1 C10 C13 121.8(3) . .
N1 C10 H10A 119.1 . .
C13 C10 H10A 119.1 . .
C13 C11 C9 120.2(3) . .
C13 C11 H11A 119.9 . .
C9 C11 H11A 119.9 . .
C10 C13 C11 118.5(3) . .
C10 C13 H13A 120.8 . .
C11 C13 H13A 120.8 . .
C7 C14 H14A 109.5 . .
C7 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C7 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O3 1.8704(6) .
Mn1 O2 1.935(2) .
Mn1 N2 2.012(2) .
Mn1 N1 2.033(2) .
Mn1 O1 2.1670(19) 3_655
Mn1 O4 2.200(2) .
Mn1 Mn1 3.2005(7) 2_545
Mn1 Mn1 3.2005(7) 3_655
O1 N2 1.314(3) .
O1 Mn1 2.1669(19) 2_545
O2 C7 1.294(4) .
O3 Mn1 1.8704(6) 2_545
O3 Mn1 1.8704(6) 3_655
O4 C7 1.240(4) 2_545
N1 C10 1.350(4) .
N1 C4 1.350(4) .
N2 C1 1.292(4) .
C1 C4 1.462(4) .
C1 C2 1.502(3) .
C2 C1 1.502(3) 6_545
C2 H2A 0.9558 .
C4 C9 1.387(4) .
C7 O4 1.240(4) 3_655
C7 C14 1.503(4) .
C9 C11 1.384(5) .
C9 H9A 0.9500 .
C10 C13 1.373(5) .
C10 H10A 0.9500 .
C11 C13 1.378(6) .
C11 H11A 0.9500 .
C13 H13A 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
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 -0.011 -0.006 -0.001 2065 1641 ' '
