#------------------------------------------------------------------------------
#$Date: 2017-05-06 01:05:16 +0300 (Sat, 06 May 2017) $
#$Revision: 196422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/24/7042457.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_7042457
loop_
_publ_author_name
'Lunsford, Allen M.'
'Goldstein, Kristina F.'
'Cohan, Matthew A.'
'Denny, Jason A.'
'Bhuvanesh, Nattamai'
'Ding, Shengda'
'Hall, Michael B.'
'Darensbourg, Marcetta Y.'
_publ_section_title
;
 Comparisons of MN2S2vs. bipyridine as redox-active ligands to manganese
 and rhenium in (L-L)M'(CO)3Cl complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5175
_journal_page_last               5182
_journal_paper_doi               10.1039/c7dt00600d
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C12 H18 Br Fe Mn N3 O4 S2'
_chemical_formula_sum            'C12 H18 Br Fe Mn N3 O4 S2'
_chemical_formula_weight         523.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6248(15)
_cell_length_b                   10.8713(9)
_cell_length_c                   9.1657(7)
_cell_measurement_reflns_used    6813
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      60.164
_cell_measurement_theta_min      4.748
_cell_volume                     1855.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.847
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22616
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         60.719
_diffrn_reflns_theta_min         4.748
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.632
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1186 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.6452.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0318P)²+6.2520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1376
_reflns_number_total             1491
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00600d3.cif
_cod_data_source_block           femnbr
_cod_depositor_comments
'Adding full bibliography for 7042451--7042457.cif.'
_cod_database_code               7042457
_shelxl_version_number           2014-3
_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_max   0.851
_shelx_estimated_absorpt_t_min   0.350
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, 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
Br1 Br 0.17623(4) 0.2500 0.80113(8) 0.0223(2) Uani 1 2 d S T P
Fe1 Fe 0.30425(6) 0.2500 0.45902(11) 0.0181(3) Uani 1 2 d S T P
Mn1 Mn 0.12876(6) 0.2500 0.54082(12) 0.0228(3) Uani 1 2 d S T P
S1 S 0.21647(6) 0.39151(12) 0.44556(12) 0.0216(3) Uani 1 1 d . . .
O2 O 0.0544(3) 0.2500 0.2598(6) 0.0421(15) Uani 1 2 d S T P
N1 N 0.3626(2) 0.3688(4) 0.5816(4) 0.0196(9) Uani 1 1 d . . .
O3 O 0.0353(2) 0.0474(4) 0.6444(4) 0.0400(10) Uani 1 1 d . . .
N2 N 0.3412(3) 0.2500 0.2905(7) 0.0232(14) Uani 1 2 d S T P
O1 O 0.3514(3) 0.2500 0.1636(6) 0.0437(15) Uani 1 2 d S T P
C3 C 0.3576(3) 0.3206(4) 0.7350(5) 0.0201(11) Uani 1 1 d . . .
H3A H 0.3130 0.3511 0.7811 0.024 Uiso 1 1 calc R . .
H3B H 0.3989 0.3511 0.7928 0.024 Uiso 1 1 calc R . .
C1 C 0.2533(3) 0.4999(5) 0.5807(5) 0.0246(12) Uani 1 1 d . . .
H1A H 0.2355 0.5841 0.5606 0.030 Uiso 1 1 calc R . .
H1B H 0.2376 0.4762 0.6800 0.030 Uiso 1 1 calc R . .
C4 C 0.4396(3) 0.3688(5) 0.5333(5) 0.0278(13) Uani 1 1 d . . .
H4A H 0.4649 0.4384 0.5802 0.033 Uiso 1 1 calc R . .
H4B H 0.4415 0.3815 0.4264 0.033 Uiso 1 1 calc R . .
C2 C 0.3339(3) 0.4972(5) 0.5715(6) 0.0266(12) Uani 1 1 d . . .
H2A H 0.3493 0.5343 0.4780 0.032 Uiso 1 1 calc R . .
H2B H 0.3543 0.5473 0.6517 0.032 Uiso 1 1 calc R . .
C5 C 0.4780(4) 0.2500 0.5710(8) 0.034(2) Uani 1 2 d S T P
H5A H 0.4877 0.2500 0.6772 0.040 Uiso 1 2 calc RS T P
H5B H 0.5250 0.2500 0.5206 0.040 Uiso 1 2 calc RS T P
C7 C 0.0707(3) 0.1264(6) 0.6040(5) 0.0308(13) Uani 1 1 d . . .
C6 C 0.0835(4) 0.2500 0.3652(9) 0.0292(18) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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
S1 Fe1 S1 86.35(7) 7_565 .
N1 Fe1 S1 148.88(12) . 7_565
N1 Fe1 S1 148.88(12) 7_565 .
N1 Fe1 S1 89.11(12) . .
N1 Fe1 S1 89.11(12) 7_565 7_565
N1 Fe1 N1 79.1(2) . 7_565
N2 Fe1 S1 104.24(14) . .
N2 Fe1 S1 104.24(14) . 7_565
N2 Fe1 N1 106.71(19) . .
N2 Fe1 N1 106.71(19) . 7_565
S1 Mn1 Br1 95.99(5) 7_565 .
S1 Mn1 Br1 95.99(5) . .
S1 Mn1 S1 79.42(7) . 7_565
C7 Mn1 Br1 84.72(16) 7_565 .
C7 Mn1 Br1 84.72(16) . .
C7 Mn1 S1 92.67(18) . 7_565
C7 Mn1 S1 172.10(18) 7_565 7_565
C7 Mn1 S1 92.68(18) 7_565 .
C7 Mn1 S1 172.10(18) . .
C7 Mn1 C7 95.2(4) . 7_565
C6 Mn1 Br1 172.7(2) . .
C6 Mn1 S1 89.61(18) . 7_565
C6 Mn1 S1 89.61(18) . .
C6 Mn1 C7 90.4(2) . 7_565
C6 Mn1 C7 90.4(2) . .
Fe1 S1 Mn1 92.08(5) . .
C1 S1 Fe1 97.47(17) . .
C1 S1 Mn1 114.68(17) . .
C3 N1 Fe1 105.2(3) . .
C4 N1 Fe1 110.4(3) . .
C4 N1 C3 109.6(4) . .
C2 N1 Fe1 111.6(3) . .
C2 N1 C3 111.1(4) . .
C2 N1 C4 108.8(4) . .
O1 N2 Fe1 165.2(6) . .
N1 C3 C3 110.4(2) . 7_565
N1 C3 H3A 109.6 . .
N1 C3 H3B 109.6 . .
C3 C3 H3A 109.6 7_565 .
C3 C3 H3B 109.6 7_565 .
H3A C3 H3B 108.1 . .
S1 C1 H1A 109.9 . .
S1 C1 H1B 109.9 . .
H1A C1 H1B 108.3 . .
C2 C1 S1 108.8(3) . .
C2 C1 H1A 109.9 . .
C2 C1 H1B 109.9 . .
N1 C4 H4A 109.1 . .
N1 C4 H4B 109.1 . .
N1 C4 C5 112.5(4) . .
H4A C4 H4B 107.8 . .
C5 C4 H4A 109.1 . .
C5 C4 H4B 109.1 . .
N1 C2 C1 111.8(4) . .
N1 C2 H2A 109.3 . .
N1 C2 H2B 109.3 . .
C1 C2 H2A 109.3 . .
C1 C2 H2B 109.3 . .
H2A C2 H2B 107.9 . .
C4 C5 C4 116.8(6) . 7_565
C4 C5 H5A 108.1 7_565 .
C4 C5 H5A 108.1 . .
C4 C5 H5B 108.1 7_565 .
C4 C5 H5B 108.1 . .
H5A C5 H5B 107.3 . .
O3 C7 Mn1 178.8(5) . .
O2 C6 Mn1 178.2(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Mn1 2.5445(13) .
Fe1 S1 2.2483(15) .
Fe1 S1 2.2483(15) 7_565
Fe1 N1 2.028(4) 7_565
Fe1 N1 2.028(4) .
Fe1 N2 1.691(6) .
Mn1 S1 2.4078(15) 7_565
Mn1 S1 2.4077(15) .
Mn1 C7 1.819(6) 7_565
Mn1 C7 1.819(6) .
Mn1 C6 1.817(9) .
S1 C1 1.843(5) .
O2 C6 1.108(9) .
N1 C3 1.503(6) .
N1 C4 1.500(6) .
N1 C2 1.498(6) .
O3 C7 1.145(6) .
N2 O1 1.179(7) .
C3 C3 1.536(9) 7_565
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.504(7) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C4 C5 1.517(7) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C5 C4 1.517(7) 7_565
C5 H5A 0.9900 .
C5 H5B 0.9900 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Fe1 S1 C1 C2 34.0(4) . .
Fe1 N1 C3 C3 36.3(2) . 7_565
Fe1 N1 C4 C5 -69.9(5) . .
Fe1 N1 C2 C1 43.3(5) . .
Mn1 S1 C1 C2 129.8(3) . .
S1 Fe1 N2 O1 44.90(5) 7_565 .
S1 Fe1 N2 O1 -44.90(6) . .
S1 C1 C2 N1 -52.0(5) . .
N1 Fe1 N2 O1 138.32(13) 7_565 .
N1 Fe1 N2 O1 -138.32(13) . .
N1 C4 C5 C4 47.6(8) . 7_565
C3 N1 C4 C5 45.5(5) . .
C3 N1 C2 C1 -73.8(5) . .
C4 N1 C3 C3 -82.4(3) . 7_565
C4 N1 C2 C1 165.4(4) . .
C2 N1 C3 C3 157.3(3) . 7_565
C2 N1 C4 C5 167.3(4) . .
