Comparisons of MN2S2vs. bipyridine as redox-active ligands to manganese and rhenium in (L-L)M'(CO)3Cl complexes.
Lunsford, Allen M.; Goldstein, Kristina F.; Cohan, Matthew A.; Denny, Jason A.; Bhuvanesh, Nattamai; Ding, Shengda; Hall, Michael B.; Darensbourg, Marcetta Y.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5175–5182; doi:10.1039/c7dt00600d

data_7042453
_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
'1.03(C11.7 H17.55 Cl0.97 N1.95 Ni0.97 O2.92 Re0.97 S1.95)'
_chemical_formula_sum            'C12 H18 Cl N2 Ni O3 Re S2'
_chemical_formula_weight         582.76
_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             2014-08-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_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                   12.2999(4)
_cell_length_b                   12.3134(4)
_cell_length_c                   10.9388(6)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      60.767
_cell_measurement_theta_min      5.409
_cell_volume                     1656.72(12)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.844
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32269
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         60.754
_diffrn_reflns_theta_min         5.409
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.433
_exptl_absorpt_correction_T_max  0.4613
_exptl_absorpt_correction_T_min  0.2122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1535 before and 0.0889 after correction.
The Ratio of minimum to maximum transmission is 0.4600.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1328
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0305
_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/[\s^2^(Fo^2^)+(0.0399P)^2^+9.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1263
_reflns_number_total             1328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00600d3.cif
_cod_data_source_block           nireb
_cod_depositor_comments
'Adding full bibliography for 7042451--7042457.cif.'
_cod_database_code               7042453
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.204
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 Re1A-O1A
 3.06 with sigma of 0.04
 C5A_$2-C5A \\sim C5_$2-C5
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Re1) = Uanis(Re1A)
Uanis(S1) = Uanis(S1A)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(Ni1) = Uanis(Ni1A)
Uanis(O1) = Uanis(O2) = Uanis(O1A) = Uanis(O2A)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C1A) = Uanis(C2A) = Uanis(C3A) = Uanis(C4A) = Uanis(C5A) =
Uanis(C6A) = Uanis(C7A)
Uanis(N1A) = Uanis(N1)
4. Same fragment restrains
{Re1, S1, Cl1, Ni1, O1, O2, N1, C1, C2, C3, C4, C5, C6, C7}
as
{Re1A, S1A, Cl1A, Ni1A, O1A, O2A, N1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A}
5. Others
 Sof(S1A)=Sof(O1A)=Sof(N1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=1-
 FVAR(1)
 Sof(Re1A)=Sof(Cl1A)=Sof(Ni1A)=Sof(O2A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C7A)=
 0.5*(1-FVAR(2))
 Sof(Re1)=Sof(Cl1)=Sof(Ni1)=Sof(O2)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C7)=0.5*
 FVAR(2)
 Sof(S1)=Sof(O1)=Sof(N1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1A(H1AA,
 H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB)
;
_shelx_res_checksum              4105