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_4346257
_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         'C56 H36 Mn4 N4 O12 S4, 2(C3 H6 O)'
_chemical_formula_sum            'C62 H48 Mn4 N4 O14 S4'
_chemical_formula_weight         1421.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.549(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5167(5)
_cell_length_b                   16.8489(8)
_cell_length_c                   16.4263(6)
_cell_measurement_reflns_used    4161
_cell_measurement_temperature    213(90)
_cell_measurement_theta_max      29.1146
_cell_measurement_theta_min      3.6759
_cell_volume                     3181.3(2)
_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      213(90)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_details
;
  1 omega  -60.00   54.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835   19.0000    0.0000 114

  2 omega  -81.00   -7.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835  141.0000  137.0000 74

  3 omega  -23.00   23.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835  -99.0000  -60.0000 46

  4 omega  -43.00  -18.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1835   37.0000   90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0032501000
_diffrn_orient_matrix_UB_12      0.0135244000
_diffrn_orient_matrix_UB_13      0.0406990000
_diffrn_orient_matrix_UB_21      -0.0022936000
_diffrn_orient_matrix_UB_22      0.0398125000
_diffrn_orient_matrix_UB_23      -0.0140208000
_diffrn_orient_matrix_UB_31      -0.0615740000
_diffrn_orient_matrix_UB_32      -0.0021941000
_diffrn_orient_matrix_UB_33      -0.0042851000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16135
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.75
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96916
_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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                4914
_reflns_number_total             7248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01118_si_002.cif
_cod_data_source_block           3
_cod_database_code               4346257
_chemical_oxdiff_formula         'C18 H14 N4 O4 S4 Mn4'
_chemical_oxdiff_usercomment     '150K, RED COLOR PLATE, 0.1 0.05 0.03'
_reflns_odcompleteness_completeness 98.96
_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.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C10(H10), C7(H7), C19(H19), C14(H14), C16(H16), C24(H24), C8(H8),
 C22(H22), C15(H15), C11(H11), C28(H28), C25(H25), C27(H27), C26(H26), C21(H21),
  C12(H12), C20(H20)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C)
;