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_4516181
_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         'C56 H64 N8 O16 Re4 S4, 4(C3 H7 N O)'
_chemical_formula_sum            'C68 H92 N12 O20 Re4 S4'
_chemical_formula_weight         2270.58
_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             2015-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                103.053(2)
_cell_angle_beta                 95.080(2)
_cell_angle_gamma                108.299(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5644(3)
_cell_length_b                   14.7817(4)
_cell_length_c                   23.8992(6)
_cell_measurement_reflns_used    11270
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      29.2217
_cell_measurement_theta_min      2.6498
_cell_volume                     4365.7(2)
_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      149.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32749
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.692
_exptl_absorpt_correction_T_max  0.203
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.943
_refine_diff_density_min         -2.161
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         15356
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0440P)^2^+56.1849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                11270
_reflns_number_total             15356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao7b02075_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        4365.65(19)
_cod_database_code               4516181
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1E-C53 = C1G-C1E = C1G-C1F
 1.53 with sigma of 0.02
 C54-C53 = C55-C54 = C55-C56
 1.53 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1F) = Uanis(C1G) = Uanis(C1E) = Uanis(C54) = Uanis(C55) = Uanis(C56)
Uanis(O18) = Uanis(O19)
Uanis(C48) = Uanis(C47)
5. Others
 Sof(H53C)=Sof(H53D)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=1-FVAR(1)
 Sof(H53A)=Sof(H53B)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=
 Sof(H1FC)=Sof(C1G)=Sof(H1GA)=Sof(H1GB)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C8(H8A,H8B), C51(H51A,H51B), C7(H7A,H7B), C41(H41A,H41B),
 C21(H21A,H21B), C49(H49A,H49B), C42(H42A,H42B), C43(H43A,H43B), C50(H50A,H50B),
  C46(H46A,H46B), C45(H45A,H45B), C47(H47A,H47B), C53(H53C,H53D), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C1E(H1EA,H1EB), C1G(H1GA,H1GB)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C11(H11), C12(H12), C1(H1), C28(H28), C16(H16), N7(H7), N8(H8),
 C5(H5A), C18(H18), C19(H19), C25(H25), C14(H14), C13(H13), C4(H4), C27(H27),
 C2(H2), N6(H6), C26(H26), C15(H15), C62(H62), C59(H59), C67(H67), C65(H65)
6.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C57(H57A,H57B,H57C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C64(H64A,
 H64B,H64C), C63(H63A,H63B,H63C), C48(H48A,H48B,H48C), C58(H58A,H58B,H58C),
 C1F(H1FA,H1FB,H1FC), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'