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_4346259
_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         '2(C60 H40 Mn4 N4 O12 S4)'
_chemical_formula_sum            'C120 H80 Mn8 N8 O24 S8'
_chemical_formula_weight         2713.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.174(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.8413(5)
_cell_length_b                   17.2727(6)
_cell_length_c                   19.2668(6)
_cell_measurement_reflns_used    7870
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      28.5421
_cell_measurement_theta_min      3.7572
_cell_volume                     6079.3(3)
_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      120.05(10)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
  1 omega  -19.00   26.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.7238  -99.0000 -120.0000 45

  2 omega -109.00  -38.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.7238 -178.0000    0.0000 71

  3 omega  -49.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1301  -19.0000  150.0000 140

  4 omega  -17.00   66.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1301   37.0000 -150.0000 83
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0014940000
_diffrn_orient_matrix_UB_12      0.0371323000
_diffrn_orient_matrix_UB_13      0.0153349000
_diffrn_orient_matrix_UB_21      0.0262810000
_diffrn_orient_matrix_UB_22      0.0139244000
_diffrn_orient_matrix_UB_23      -0.0177503000
_diffrn_orient_matrix_UB_31      -0.0285495000
_diffrn_orient_matrix_UB_32      0.0107251000
_diffrn_orient_matrix_UB_33      -0.0298473000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32149
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62524
_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 dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_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             2752
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0492P)^2^+8.5263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                7907
_reflns_number_total             13542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01118_si_002.cif
_cod_data_source_block           5
_cod_database_code               4346259
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C30A) =
Uanis(C29A) = Uanis(C28A) = Uanis(C27A) = Uanis(C26A)
Uanis(C49) = Uanis(C49A)
Uanis(C55A) = Uanis(C60A) = Uanis(C59A) = Uanis(C58A) = Uanis(C57A) =
Uanis(C56A) = Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) =
Uanis(C60)
3. Others
 Sof(O13)=Sof(C1B)=Sof(C1C)=Sof(O19)=1-FVAR(1)
 Sof(O11)=Sof(O12)=Sof(C36)=Sof(C35)=FVAR(1)
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=
 Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(2)
 Sof(C27)=Sof(H27)=Sof(C26)=Sof(H26)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=
 Sof(C30)=Sof(H30)=FVAR(2)
 Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=Sof(C51A)=
 Sof(H51A)=Sof(C50A)=Sof(H50A)=1-FVAR(3)
 Sof(C54)=Sof(H54)=Sof(C50)=Sof(H50)=Sof(C52)=Sof(H52)=Sof(C51)=Sof(H51)=
 Sof(C53)=Sof(H53)=FVAR(3)
 Sof(C49A)=1-FVAR(4)
 Sof(C49)=FVAR(4)
 Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=Sof(C60A)=Sof(H60A)=1-FVAR(5)
 Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=
 Sof(C60)=Sof(H60)=FVAR(5)
 Sof(C55A)=1-FVAR(6)
 Sof(C55)=FVAR(6)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C42(H42), C13(H13), C37(H37), C38(H38), C17(H17), C41(H41),
 C10(H10), C46(H46), C43(H43), C11(H11), C18(H18), C45(H45), C15(H15), C7(H7),
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C48(H48), C40(H40),
  C16(H16), C47(H47), C20(H20), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C21(H21), C24(H24), C22(H22), C27(H27), C26(H26), C28(H28), C23(H23),
  C54(H54), C50(H50), C52(H52), C51(H51), C53(H53), C29(H29), C30(H30),
 C54A(H54A), C53A(H53A), C52A(H52A), C51A(H51A), C50A(H50A), C56A(H56A),
 C57A(H57A), C58A(H58A), C59A(H59A), C60A(H60A)
4.b Fitted hexagon refined as free rotating group:
 C25(C26A,C27A,C28A,C29A,C30A), C55(C56,C57,C58,C59,C60), C55A(C56A,C57A,C58A,
 C59A,C60A)
;
_olex2_submission_special_instructions 'No special instructions were received'