Self-assembly of Thiolato-Bridged Manganese(I)-Based Metallarectangles: One-pot Synthesis and Structural Characterization.
Ashok Kumar, Chowan; Nagarajaprakash, R.; Ramakrishna, Buthanapalli; Manimaran, Bala; Inorganic chemistry 54 (2015) 8406–8414; doi:10.1021/acs.inorgchem.5b01118

data_4346256
_publ_section_title
;
 Self-assembly of Thiolato-Bridged Manganese(I)-Based Metallarectangles:
 One-pot Synthesis and Structural Characterization.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8406
_journal_page_last               8414
_journal_paper_doi               10.1021/acs.inorgchem.5b01118
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C44 H28 Mn4 N4 O12 S4, 2(C3 H6 O)'
_chemical_formula_sum            'C50 H40 Mn4 N4 O14 S4'
_chemical_formula_weight         1268.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                75.925(5)
_cell_angle_beta                 87.244(4)
_cell_angle_gamma                69.475(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1720(4)
_cell_length_b                   11.5283(7)
_cell_length_c                   14.0257(7)
_cell_measurement_reflns_used    3492
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      29.0861
_cell_measurement_theta_min      3.5535
_cell_volume                     1346.07(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -54.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000  -30.0000 55

  2 omega  -12.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000 -150.0000 37

  3 omega  -66.00   10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -19.0000 -180.0000 76

  4 omega  -81.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000   90.0000 61

  5 omega  -77.00   -8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000  150.0000 69

  6 omega  -74.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000  -60.0000 76

  7 omega  -67.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  113.0000  111.0000 47

  8 omega   32.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9803 -178.0000   30.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0233177000
_diffrn_orient_matrix_UB_12      -0.0532891000
_diffrn_orient_matrix_UB_13      -0.0213827000
_diffrn_orient_matrix_UB_21      0.0294146000
_diffrn_orient_matrix_UB_22      -0.0413709000
_diffrn_orient_matrix_UB_23      0.0466918000
_diffrn_orient_matrix_UB_31      -0.0737402000
_diffrn_orient_matrix_UB_32      -0.0067560000
_diffrn_orient_matrix_UB_33      0.0094631000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10876
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+3.9544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                3805
_reflns_number_total             4704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01118_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        1346.07(12)
_cod_database_code               4346256
_chemical_oxdiff_usercomment     '150K, RED COLOR PLATE, 0.38 0.18 0.03'
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C11) = Uanis(C15) = Uanis(C13) = Uanis(C12) = Uanis(C16)
Uanis(O7) = Uanis(O8)
3. Others
 Sof(O7)=Sof(C24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=
 Sof(H1CC)=Sof(O8)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C13(H13), C15(H15), C14(H14), C12(H12), C22(H22),
 C18(H18), C21(H21), C19(H19), C20(H20), C10(H10), C8(H8)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C1A(H1AA,H1AB,H1AC), C1C(H1CA,H1CB,
 H1CC)
;