One-pot synthesis of oxamidato-bridged hexarhenium trigonal prisms adorned with ester functionality.
Nagarajaprakash, R.; Govindarajan, R.; Manimaran, Bala; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11732–11740; doi:10.1039/c5dt01102g

data_7702028
_publ_section_title
;
 One-pot synthesis of oxamidato-bridged hexarhenium trigonal prisms
 adorned with ester functionality.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11732
_journal_page_last               11740
_journal_paper_doi               10.1039/c5dt01102g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C114 H72 N12 O36 Re6'
_chemical_formula_sum            'C114 H72 N12 O36 Re6'
_chemical_formula_weight         3303.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yac'
_space_group_name_H-M_alt        'C 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-18 deposited with the CCDC.
2015-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.403(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.648(2)
_cell_length_b                   27.6088(13)
_cell_length_c                   14.0477(9)
_cell_measurement_temperature    150
_cell_volume                     13172.6(13)
_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      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28381
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.40396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6326
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         2.275
_refine_diff_density_min         -2.298
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         11593
_refine_ls_number_restraints     821
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                6916
_reflns_number_total             11593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt01102g2.cif
_cod_data_source_block           4
_cod_original_cell_volume        13172.7(13)
_cod_original_sg_symbol_Hall     '-C 2ybc'
_cod_original_sg_symbol_H-M      'C 2/n'
_cod_database_code               7702028
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O14A-C4
 1.28 with sigma of 0.02
 N1-C9
 1.5 with sigma of 0.02
 O5-C4 = N1A-C4 = N1-C4 = N3-C5 = O15A-C5 = O4-C5 = N3A-C5
 1.28 with sigma of 0.02
 Re2_$1-O5_$1
 2.123 with sigma of 0.02
 C3-Re1
 1.912 with sigma of 0.02
3. Restrained planarity
 N4A, C53A, C54A, C55A, C56A, C57A
 with sigma of 0.1
 N4, C53, C54, C55, C56, C57
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C57) = Uanis(C57A)
Uanis(N4) = Uanis(N4A)
Uanis(C56) = Uanis(C56A)
Uanis(C54) = Uanis(C54A)
Uanis(C53) = Uanis(C53A)
Uanis(C15A) = Uanis(C14A)
Uanis(C55) = Uanis(C11)
Uanis(O14A) = Uanis(N1)
Uanis(C13) = Uanis(C14)
Uanis(C3) = Uanis(O3)
5. Others
 Sof(C35A)=Sof(O11A)=Sof(N4A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=1-FVAR(1)
 Sof(N4)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(C56)=Sof(H56)=
 Sof(C57)=Sof(H57)=Sof(O12)=Sof(O12A)=Sof(C35)=Sof(O11)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=
 Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=
 Sof(H21A)=Sof(C20A)=Sof(H20A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=
 Sof(O15A)=Sof(N3A)=Sof(N1A)=Sof(O14A)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(N3)=Sof(O4)=Sof(N1)=Sof(O5)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C46(H46B,H46C), C9A(H9AA,H9AB), C9(H9A,H9B), C16(H16A,H16B), C16A(H16C,H16D)
6.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C34(H34), C32(H32), C40(H40), C41(H41), C53(H53), C54(H54),
 C56(H56), C57(H57), C52(H52), C51(H51), C50(H50), C49(H49), C48(H48), C39(H39),
  C38(H38), C23(H23), C26(H26), C24(H24), C27(H27), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C53A(H53A),
 C54A(H54A), C56A(H56A), C57A(H57A), C22A(H22A), C21A(H21A), C20A(H20A),
 C19A(H19A), C18A(H18A)
6.c Fitted hexagon refined as free rotating group:
 C47(C52,C51,C50,C49,C48), C10A(C11A,C12A,C13A,C14A,C15A), C10(C11,C12,C13,C14,
 C15), C17(C18,C19,C20,C21,C22), C17A(C22A,C21A,C20A,C19A,C18A)
;
_olex2_submission_special_instructions 'No special instructions were received'