#------------------------------------------------------------------------------
#$Date: 2017-05-06 01:05:16 +0300 (Sat, 06 May 2017) $
#$Revision: 196422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/24/7042454.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_7042454
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 Cl Fe N3 O4 Re S2'
_chemical_formula_sum            'C12 H18 Cl Fe N3 O4 Re S2'
_chemical_formula_weight         609.91
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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                   18.8370(8)
_cell_length_b                   10.3101(4)
_cell_length_c                   9.3359(4)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      32.047
_cell_measurement_theta_min      3.911
_cell_volume                     1813.14(13)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30754
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.446
_diffrn_reflns_theta_min         3.653
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.869
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1569 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.4129.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.432
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         3304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0240
_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)+(0.0169P)²+2.2044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2977
_reflns_number_total             3304
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00600d3.cif
_cod_data_source_block           fenore
_cod_depositor_comments
'Adding full bibliography for 7042451--7042457.cif.'
_cod_database_code               7042454
_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   0.507
_shelx_estimated_absorpt_t_min   0.244
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B), C2(H2A,H2B)
;
_shelx_shelxl_version_number     2014/7
_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
Re1 Re 0.12411(2) 0.2500 0.45848(2) 0.01392(5) Uani 1 2 d S T P
Fe1 Fe 0.30434(3) 0.2500 0.54197(5) 0.01297(9) Uani 1 2 d S T P
Cl1 Cl 0.18095(4) 0.2500 0.21612(8) 0.01745(15) Uani 1 2 d S T P
S1 S 0.21754(3) 0.39990(6) 0.55680(6) 0.01490(11) Uani 1 1 d . . .
O2 O 0.04774(16) 0.2500 0.7469(3) 0.0310(7) Uani 1 2 d S T P
O3 O 0.02644(12) 0.0343(2) 0.3468(2) 0.0342(5) Uani 1 1 d . . .
C7 C 0.06233(14) 0.1152(3) 0.3907(3) 0.0202(5) Uani 1 1 d . . .
C6 C 0.0767(2) 0.2500 0.6387(4) 0.0214(7) Uani 1 2 d S T P
N1 N 0.36093(12) 0.3752(2) 0.4209(2) 0.0171(4) Uani 1 1 d . . .
O1 O 0.3611(2) 0.2500 0.8242(4) 0.0463(9) Uani 1 2 d S T P
N2 N 0.34291(16) 0.2500 0.7050(3) 0.0186(6) Uani 1 2 d S T P
C1 C 0.25335(15) 0.5134(2) 0.4243(3) 0.0201(5) Uani 1 1 d . . .
H1A H 0.2376 0.4882 0.3270 0.024 Uiso 1 1 calc R . .
H1B H 0.2358 0.6022 0.4442 0.024 Uiso 1 1 calc R . .
C4 C 0.4753(2) 0.2500 0.4267(4) 0.0278(9) Uani 1 2 d S T P
H4A H 0.5222 0.2500 0.4745 0.033 Uiso 1 2 calc RS T P
H4B H 0.4839 0.2500 0.3221 0.033 Uiso 1 2 calc RS T P
C5 C 0.35496(14) 0.3250(2) 0.2712(2) 0.0163(4) Uani 1 1 d . . .
H5A H 0.3953 0.3572 0.2135 0.020 Uiso 1 1 calc R . .
H5B H 0.3105 0.3572 0.2272 0.020 Uiso 1 1 calc R . .
C3 C 0.43730(15) 0.3747(3) 0.4656(3) 0.0253(6) Uani 1 1 d . . .
H3A H 0.4400 0.3875 0.5706 0.030 Uiso 1 1 calc R . .
H3B H 0.4619 0.4484 0.4193 0.030 Uiso 1 1 calc R . .
C2 C 0.33308(15) 0.5106(3) 0.4326(3) 0.0216(5) Uani 1 1 d . . .
H2A H 0.3531 0.5640 0.3543 0.026 Uiso 1 1 calc R . .
H2B H 0.3486 0.5488 0.5248 0.026 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Cl1 Re1 S1 91.75(2) . 7_565
Cl1 Re1 S1 91.75(2) . .
S1 Re1 S1 75.81(3) 7_565 .
C7 Re1 Cl1 87.78(8) 7_565 .
C7 Re1 Cl1 87.78(8) . .
C7 Re1 S1 171.49(8) . .
C7 Re1 S1 171.49(8) 7_565 7_565
C7 Re1 S1 95.71(8) . 7_565
C7 Re1 S1 95.71(8) 7_565 .
C7 Re1 C7 92.76(15) 7_565 .
C6 Re1 Cl1 177.35(11) . .
C6 Re1 S1 90.34(9) . 7_565
C6 Re1 S1 90.34(9) . .
C6 Re1 C7 90.40(11) . 7_565
C6 Re1 C7 90.40(11) . .
S1 Fe1 S1 86.57(4) . 7_565
N1 Fe1 S1 148.79(7) 7_565 .
N1 Fe1 S1 88.80(7) . .
N1 Fe1 S1 148.79(7) . 7_565
N1 Fe1 S1 88.80(7) 7_565 7_565
N1 Fe1 N1 79.43(13) 7_565 .
N2 Fe1 S1 104.89(8) . 7_565
N2 Fe1 S1 104.89(8) . .
N2 Fe1 N1 106.12(10) . 7_565
N2 Fe1 N1 106.12(10) . .
Fe1 S1 Re1 93.66(2) . .
C1 S1 Re1 113.81(9) . .
C1 S1 Fe1 97.45(9) . .
O3 C7 Re1 178.2(2) . .
O2 C6 Re1 179.6(3) . .
C5 N1 Fe1 105.21(15) . .
C5 N1 C3 109.4(2) . .
C5 N1 C2 111.4(2) . .
C3 N1 Fe1 110.42(17) . .
C2 N1 Fe1 111.75(16) . .
C2 N1 C3 108.6(2) . .
O1 N2 Fe1 171.6(3) . .
S1 C1 H1A 110.0 . .
S1 C1 H1B 110.0 . .
H1A C1 H1B 108.3 . .
C2 C1 S1 108.67(18) . .
C2 C1 H1A 110.0 . .
C2 C1 H1B 110.0 . .
H4A C4 H4B 107.4 . .
C3 C4 H4A 108.3 . .
C3 C4 H4A 108.3 7_565 .
C3 C4 H4B 108.3 7_565 .
C3 C4 H4B 108.3 . .
C3 C4 C3 116.0(3) . 7_565
N1 C5 C5 110.25(13) . 7_565
N1 C5 H5A 109.6 . .
N1 C5 H5B 109.6 . .
C5 C5 H5A 109.6 7_565 .
C5 C5 H5B 109.6 7_565 .
H5A C5 H5B 108.1 . .
N1 C3 C4 112.9(2) . .
N1 C3 H3A 109.0 . .
N1 C3 H3B 109.0 . .
C4 C3 H3A 109.0 . .
C4 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
N1 C2 C1 111.4(2) . .
N1 C2 H2A 109.4 . .
N1 C2 H2B 109.4 . .
C1 C2 H2A 109.4 . .
C1 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Cl1 2.5032(8) .
Re1 S1 2.5157(6) 7_565
Re1 S1 2.5157(6) .
Re1 C7 1.920(3) 7_565
Re1 C7 1.920(3) .
Re1 C6 1.905(4) .
Fe1 S1 2.2541(7) .
Fe1 S1 2.2541(7) 7_565
Fe1 N1 2.020(2) .
Fe1 N1 2.020(2) 7_565
Fe1 N2 1.687(3) .
S1 C1 1.832(3) .
O2 C6 1.148(5) .
O3 C7 1.148(3) .
N1 C5 1.494(3) .
N1 C3 1.498(3) .
N1 C2 1.495(4) .
O1 N2 1.164(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.504(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C4 C3 1.516(4) 7_565
C4 C3 1.516(4) .
C5 C5 1.546(5) 7_565
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 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
Re1 S1 C1 C2 -131.66(15) . .
Fe1 S1 C1 C2 -34.30(18) . .
Fe1 N1 C5 C5 -36.27(13) . 7_565
Fe1 N1 C3 C4 70.0(3) . .
Fe1 N1 C2 C1 -44.1(2) . .
S1 C1 C2 N1 52.7(2) . .
C5 N1 C3 C4 -45.3(3) . .
C5 N1 C2 C1 73.2(3) . .
C3 N1 C5 C5 82.33(19) . 7_565
C3 N1 C2 C1 -166.2(2) . .
C3 C4 C3 N1 -47.9(4) 7_565 .
C2 N1 C5 C5 -157.55(15) . 7_565
C2 N1 C3 C4 -167.1(2) . .
