Amide-Functionalized Chalcogen-Bridged Flexible Tetranuclear Rhenacycles: Synthesis, Characterization, Solvent Effect on the Structure, and Guest Binding.
Karthikeyan, Muthuraman; Ramakrishna, Buthanapalli; Vellaiyadevan, Sivalingam; Divya, Dhanaraj; Manimaran, Bala; ACS omega 3 (2018) 3257–3266; doi:10.1021/acsomega.7b02075

data_4516184
_publ_section_title
;
 Amide-Functionalized Chalcogen-Bridged Flexible Tetranuclear Rhenacycles:
 Synthesis, Characterization, Solvent Effect on the Structure, and Guest
 Binding.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              3257
_journal_page_last               3266
_journal_paper_doi               10.1021/acsomega.7b02075
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C80 H64 Fe4 N8 O16 Re4 S4, 4(C3 H7 N O)'
_chemical_formula_sum            'C92 H92 Fe4 N12 O20 Re4 S4'
_chemical_formula_weight         2782.22
_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             2014-04-12
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                71.743(3)
_cell_angle_beta                 78.559(3)
_cell_angle_gamma                80.466(3)
_cell_formula_units_Z            1
_cell_length_a                   13.8133(4)
_cell_length_b                   13.9339(5)
_cell_length_c                   14.4964(5)
_cell_measurement_reflns_used    6693
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      29.0413
_cell_measurement_theta_min      3.5555
_cell_volume                     2580.96(16)
_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
;
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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9921
_diffrn_measured_fraction_theta_max 0.9280
_diffrn_measurement_details
;
  1 omega  -22.00   23.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000 -180.0000 45

  2 omega  -89.00    7.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000    0.0000 96

  3 omega  -39.00   35.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000  -60.0000 74

  4 omega  -46.00   13.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000  -30.0000 59

  5 omega  -43.00   54.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   37.0000 -180.0000 97

  6 omega  -86.00  -57.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -57.0000 -120.0000 29

  7 omega  -39.00   51.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397   57.0000   30.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0250430000
_diffrn_orient_matrix_UB_12      -0.0378899000
_diffrn_orient_matrix_UB_13      -0.0055587000
_diffrn_orient_matrix_UB_21      -0.0013718000
_diffrn_orient_matrix_UB_22      0.0278126000
_diffrn_orient_matrix_UB_23      -0.0500104000
_diffrn_orient_matrix_UB_31      0.0463684000
_diffrn_orient_matrix_UB_32      -0.0264590000
_diffrn_orient_matrix_UB_33      -0.0137565000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24588
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38328
_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_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.109
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         11776
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+5.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                8633
_reflns_number_total             11776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao7b02075_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2580.96(14)
_cod_database_code               4516184
_chemical_oxdiff_formula         'C40 H40 Fe4 Re2 S4'
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'