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_4516183
_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         'C68 H56 N8 O16 Re4 S4, 2(C3 H7 N O)'
_chemical_formula_sum            'C74 H70 N10 O18 Re4 S4'
_chemical_formula_weight         2260.44
_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 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                79.388(5)
_cell_angle_beta                 82.079(5)
_cell_angle_gamma                84.365(5)
_cell_formula_units_Z            2
_cell_length_a                   14.2470(9)
_cell_length_b                   14.3139(7)
_cell_length_c                   25.3456(14)
_cell_measurement_reflns_used    23529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.350
_cell_measurement_theta_min      2.5843
_cell_volume                     5017.8(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.853
_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  0.1024
_diffrn_reflns_av_unetI/netI     0.2481
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52257
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.951
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2184
_platon_squeeze_details
;
;
_refine_diff_density_max         3.211
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         23529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2575
_reflns_number_gt                8703
_reflns_number_total             27579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao7b02075_si_002.cif
_cod_data_source_block           2-DMF
_cod_original_cell_volume        5017.7(5)
_cod_database_code               4516183
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C50) = Uanis(C49) = Uanis(C54) = Uanis(C53) = Uanis(C52) = Uanis(C51) =
Uanis(C42) = Uanis(C47) = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43) =
Uanis(C59) = Uanis(C58) = Uanis(C57) = Uanis(C60) = Uanis(C61) = Uanis(C67) =
Uanis(C66) = Uanis(C65) = Uanis(C64) = Uanis(C68)
Uanis(C11) = Uanis(C12)
Uanis(C7) = Uanis(C9) = Uanis(C8)
Uanis(C71) = Uanis(C73) = Uanis(C72)
Uanis(C3) = Uanis(O3) = Uanis(C1) = Uanis(O1) = Uanis(C2) = Uanis(O2)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C41(H41A,H41B), C48(H48A,H48B), C55(H55A,H55B), C34(H34A,
 H34B), C33(H33A,H33B), C19(H19A,H19B), C62(H62A,H62B)
3.b Aromatic/amide H refined with riding coordinates:
 C40(H40), N4(H4), C24(H24), C13(H13), C31(H31), C38(H38), C23(H23), C14(H14),
 C17(H17), C37(H37), C30(H30), C46(H46), C39(H39), C57(H57), C58(H58), C59(H59),
  C60(H60), C61(H61), C26(H26), C25(H25), C50(H50), C51(H51), C27(H27),
 C53(H53), C28(H28), C47(H47), C54(H54), C44(H44), C52(H52), C43(H43), N5(H5),
 N3(H3), C16(H16), N6(H6), C74(H74), C45(H45), C64(H64), C67(H67), C70(H70),
 C65(H65), C66(H66), C68(H68)
3.c Fitted hexagon refined as free rotating group:
 C56(C57,C58,C59,C60,C61)
3.d Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C72(H72A,H72B,H72C), C71(H71A,H71B,H71C), C69(H69A,H69B,
 H69C)
;