#------------------------------------------------------------------------------
#$Date: 2020-05-05 16:25:32 +0300 (Tue, 05 May 2020) $
#$Revision: 251645 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/37/7703716.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7703716
loop_
_publ_author_name
'Wiratpruk, Nuchareenat'
'Noor, Asif'
'McLean, Catriona A.'
'Donnelly, Paul S.'
'Barnard, Peter J.'
_publ_section_title
;
 Charge neutral rhenium tricarbonyl complexes of tridentate N-heterocyclic
 carbene ligands that bind to amyloid plaques of Alzheimer's disease.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4559
_journal_page_last               4569
_journal_paper_doi               10.1039/c9dt04687a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H27 N6 O6 Re S'
_chemical_formula_sum            'C28 H27 N6 O6 Re S'
_chemical_formula_weight         761.81
_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     heavy
_audit_creation_date             2020-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-24 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                91.5713(19)
_cell_angle_beta                 93.4633(18)
_cell_angle_gamma                108.3622(16)
_cell_formula_units_Z            2
_cell_length_a                   7.20011(12)
_cell_length_b                   7.20961(14)
_cell_length_c                   27.7581(7)
_cell_measurement_reflns_used    7476
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.0190
_cell_measurement_theta_min      4.7740
_cell_volume                     1363.42(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            8184
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.086
_diffrn_reflns_theta_max         65.086
_diffrn_reflns_theta_min         4.794
_exptl_absorpt_coefficient_mu    9.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.112
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         8184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0951P)²+4.4104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7992
_reflns_number_total             8184
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt04687a2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7703716--7703717.cif.'
_cod_database_code               7703716
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.755
_shelx_estimated_absorpt_t_min   0.693
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6196(12)
 0.3804(12)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C5(H5), C6(H6), C15(H15), C18(H18), C19(H19), C22(H22), C23(H23),
 C25(H25), C26(H26)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4492(13) 0.5097(13) 0.5904(3) 0.0286(17) Uani 1 1 d . . . . .
N1 N 0.4150(12) 0.3296(11) 0.6068(3) 0.0357(17) Uani 1 1 d . . . . .
O1 O 0.4193(9) 0.8262(9) 0.6541(2) 0.0309(13) Uani 1 1 d . . . . .
Re1 Re 0.66612(5) 0.76899(5) 0.62522(2) 0.02458(14) Uani 1 1 d . . . . .
S1 S 1.5668(3) 0.8042(4) 0.93318(7) 0.0320(5) Uani 1 1 d . . . . .
C2 C 0.8591(14) 1.0043(15) 0.6565(3) 0.034(2) Uani 1 1 d . . . . .
N2 N 0.3265(10) 0.4830(11) 0.5498(2) 0.0284(16) Uani 1 1 d . . . . .
O2 O 0.2807(9) 0.8618(10) 0.7216(2) 0.0390(15) Uani 1 1 d . . . . .
C3 C 0.6876(12) 0.9253(14) 0.5698(3) 0.0323(19) Uani 1 1 d . . . . .
N3 N 0.6306(10) 0.6139(11) 0.6965(2) 0.0251(14) Uani 1 1 d . . . . .
O3 O 0.9733(10) 1.1446(11) 0.6715(2) 0.0447(17) Uani 1 1 d . . . . .
C4 C 0.8684(14) 0.6825(16) 0.6028(3) 0.038(2) Uani 1 1 d . . . . .
N4 N 1.0090(10) 0.6746(11) 0.7948(2) 0.0292(15) Uani 1 1 d . . . . .
H4 H 1.0973 0.7474 0.7768 0.035 Uiso 1 1 calc R . . . .
O4 O 0.7123(11) 1.0301(11) 0.5388(2) 0.0459(18) Uani 1 1 d . . . . .
C5 C 0.2689(14) 0.1925(15) 0.5772(4) 0.039(2) Uani 1 1 d . . . . .
H5 H 0.2175 0.0558 0.5812 0.047 Uiso 1 1 calc R . . . .
N5 N 1.2786(10) 0.6880(11) 0.9883(3) 0.0305(16) Uani 1 1 d . . . . .
O5 O 0.9917(11) 0.6247(13) 0.5887(3) 0.052(2) Uani 1 1 d . . . . .
C6 C 0.2162(13) 0.2931(15) 0.5420(3) 0.036(2) Uani 1 1 d . . . . .
H6 H 0.1190 0.2408 0.5162 0.043 Uiso 1 1 calc R . . . .
N6 N 1.9516(12) 0.8187(13) 1.1623(3) 0.0401(19) Uani 1 1 d . . . . .
O6 O 0.6938(10) 0.4735(12) 0.7911(2) 0.0502(19) Uani 1 1 d . . . . .
C7 C 0.3100(13) 0.6376(15) 0.5186(3) 0.034(2) Uani 1 1 d . . . . .
H7A H 0.3022 0.7490 0.5385 0.051 Uiso 1 1 calc GR . . . .
H7B H 0.1914 0.5880 0.4967 0.051 Uiso 1 1 calc GR . . . .
H7C H 0.4254 0.6797 0.4997 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.5066(16) 0.2875(16) 0.6518(3) 0.043(2) Uani 1 1 d . . . . .
H8A H 0.6482 0.3118 0.6484 0.052 Uiso 1 1 calc R . . . .
H8B H 0.4468 0.1477 0.6584 0.052 Uiso 1 1 calc R . . . .
C9 C 0.4810(13) 0.4134(13) 0.6938(3) 0.035(2) Uani 1 1 d . . . . .
H9A H 0.3479 0.4258 0.6904 0.042 Uiso 1 1 calc R . . . .
H9B H 0.4928 0.3485 0.7243 0.042 Uiso 1 1 calc R . . . .
C10 C 0.4016(13) 0.8135(13) 0.7000(3) 0.0291(18) Uani 1 1 d . . . . .
C11 C 0.5535(13) 0.7425(13) 0.7276(3) 0.0301(18) Uani 1 1 d . . . . .
H11A H 0.6641 0.8570 0.7406 0.036 Uiso 1 1 calc R . . . .
H11B H 0.4934 0.6687 0.7553 0.036 Uiso 1 1 calc R . . . .
C12 C 0.8261(12) 0.6112(14) 0.7177(3) 0.0313(19) Uani 1 1 d . . . . .
H12A H 0.9262 0.7369 0.7117 0.038 Uiso 1 1 calc R . . . .
H12B H 0.8613 0.5058 0.7007 0.038 Uiso 1 1 calc R . . . .
C13 C 0.8342(13) 0.5793(14) 0.7724(3) 0.0321(19) Uani 1 1 d . . . . .
C14 C 1.0699(12) 0.6728(13) 0.8447(3) 0.0286(18) Uani 1 1 d . . . . .
C15 C 1.2691(12) 0.7352(14) 0.8575(3) 0.0295(18) Uani 1 1 d . . . . .
H15 H 1.3613 0.7745 0.8336 0.035 Uiso 1 1 calc R . . . .
C16 C 1.3317(11) 0.7393(12) 0.9061(3) 0.0254(17) Uani 1 1 d . . . . .
C17 C 1.1970(13) 0.6788(13) 0.9417(3) 0.0290(18) Uani 1 1 d . . . . .
C18 C 0.9962(13) 0.6159(14) 0.9278(3) 0.0325(19) Uani 1 1 d . . . . .
H18 H 0.9035 0.5755 0.9514 0.039 Uiso 1 1 calc R . . . .
C19 C 0.9323(14) 0.6124(15) 0.8797(3) 0.0327(19) Uani 1 1 d . . . . .
H19 H 0.7959 0.5692 0.8703 0.039 Uiso 1 1 calc R . . . .
C20 C 1.4679(12) 0.7491(12) 0.9894(3) 0.0263(17) Uani 1 1 d . . . . .
C21 C 1.5979(12) 0.7715(12) 1.0338(3) 0.0274(17) Uani 1 1 d . . . . .
C22 C 1.7994(13) 0.8265(14) 1.0337(3) 0.034(2) Uani 1 1 d . . . . .
H22 H 1.8583 0.8534 1.0039 0.041 Uiso 1 1 calc R . . . .
C23 C 1.9174(14) 0.8434(15) 1.0754(3) 0.036(2) Uani 1 1 d . . . . .
H23 H 2.0558 0.8823 1.0740 0.043 Uiso 1 1 calc R . . . .
C24 C 1.8349(12) 0.8036(12) 1.1203(3) 0.0276(17) Uani 1 1 d . . . . .
C25 C 1.6292(14) 0.7460(14) 1.1204(3) 0.035(2) Uani 1 1 d . . . . .
H25 H 1.5687 0.7160 1.1500 0.042 Uiso 1 1 calc R . . . .
C26 C 1.5154(13) 0.7329(13) 1.0783(3) 0.0312(19) Uani 1 1 d . . . . .
H26 H 1.3769 0.6966 1.0793 0.037 Uiso 1 1 calc R . . . .
C27 C 2.1609(15) 0.9023(17) 1.1634(3) 0.043(2) Uani 1 1 d . . . . .
H27A H 2.2103 0.8435 1.1368 0.064 Uiso 1 1 calc GR . . . .
H27B H 2.2196 0.8766 1.1943 0.064 Uiso 1 1 calc GR . . . .
H27C H 2.1959 1.0438 1.1600 0.064 Uiso 1 1 calc GR . . . .
C28 C 1.8633(15) 0.7732(17) 1.2076(3) 0.042(2) Uani 1 1 d . . . . .
H28A H 1.7944 0.8666 1.2153 0.063 Uiso 1 1 calc GR . . . .
H28B H 1.9658 0.7819 1.2333 0.063 Uiso 1 1 calc GR . . . .
H28C H 1.7699 0.6403 1.2050 0.063 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Re1 123.3(6) . . ?
N1 C1 N2 104.4(7) . . ?
N2 C1 Re1 132.3(6) . . ?
C1 N1 C5 110.6(8) . . ?
C1 N1 C8 124.0(8) . . ?
C5 N1 C8 125.1(8) . . ?
C10 O1 Re1 118.1(5) . . ?
C1 Re1 N3 88.6(3) . . ?
O1 Re1 C1 85.0(3) . . ?
O1 Re1 N3 75.7(2) . . ?
C2 Re1 C1 179.3(3) . . ?
C2 Re1 O1 94.4(3) . . ?
C2 Re1 N3 91.6(3) . . ?
C3 Re1 C1 95.5(3) . . ?
C3 Re1 O1 98.6(3) . . ?
C3 Re1 C2 84.2(4) . . ?
C3 Re1 N3 172.6(3) . . ?
C4 Re1 C1 89.7(4) . . ?
C4 Re1 O1 171.9(3) . . ?
C4 Re1 C2 91.0(4) . . ?
C4 Re1 C3 88.0(4) . . ?
C4 Re1 N3 98.2(3) . . ?
C16 S1 C20 89.2(4) . . ?
O3 C2 Re1 175.2(7) . . ?
C1 N2 C7 125.2(7) . . ?
C6 N2 C1 111.5(8) . . ?
C6 N2 C7 123.3(7) . . ?
O4 C3 Re1 174.5(8) . . ?
C9 N3 Re1 115.0(5) . . ?
C11 N3 Re1 102.6(5) . . ?
C11 N3 C9 106.9(7) . . ?
C12 N3 Re1 110.1(5) . . ?
C12 N3 C9 111.6(7) . . ?
C12 N3 C11 110.1(6) . . ?
O5 C4 Re1 178.6(9) . . ?
C13 N4 C14 127.8(7) . . ?
C6 C5 N1 106.0(9) . . ?
C20 N5 C17 111.0(7) . . ?
C5 C6 N2 107.5(8) . . ?
C24 N6 C27 121.6(7) . . ?
C24 N6 C28 120.0(8) . . ?
C27 N6 C28 118.0(8) . . ?
N1 C8 C9 111.2(8) . . ?
N3 C9 C8 112.1(7) . . ?
O1 C10 C11 115.2(7) . . ?
O2 C10 O1 124.7(8) . . ?
O2 C10 C11 120.0(7) . . ?
N3 C11 C10 112.3(6) . . ?
N3 C12 C13 114.4(7) . . ?
N4 C13 C12 112.8(7) . . ?
O6 C13 N4 125.8(8) . . ?
O6 C13 C12 121.3(8) . . ?
C15 C14 N4 117.5(7) . . ?
C15 C14 C19 121.2(8) . . ?
C19 C14 N4 121.3(8) . . ?
C14 C15 C16 118.4(7) . . ?
C15 C16 S1 129.6(6) . . ?
C15 C16 C17 121.5(8) . . ?
C17 C16 S1 108.9(6) . . ?
N5 C17 C16 115.5(8) . . ?
N5 C17 C18 125.6(7) . . ?
C18 C17 C16 118.9(7) . . ?
C19 C18 C17 120.2(8) . . ?
C18 C19 C14 119.8(8) . . ?
N5 C20 S1 115.3(6) . . ?
N5 C20 C21 124.1(7) . . ?
C21 C20 S1 120.5(6) . . ?
C22 C21 C20 123.0(7) . . ?
C22 C21 C26 117.6(8) . . ?
C26 C21 C20 119.3(8) . . ?
C23 C22 C21 122.0(8) . . ?
C22 C23 C24 120.6(8) . . ?
N6 C24 C23 121.1(8) . . ?
N6 C24 C25 121.4(8) . . ?
C25 C24 C23 117.5(8) . . ?
C26 C25 C24 120.5(8) . . ?
C25 C26 C21 121.7(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.341(11) . ?
C1 Re1 2.179(9) . ?
C1 N2 1.358(11) . ?
N1 C5 1.398(12) . ?
N1 C8 1.462(12) . ?
O1 Re1 2.142(6) . ?
O1 C10 1.290(10) . ?
Re1 C2 1.963(10) . ?
Re1 C3 1.916(9) . ?
Re1 N3 2.287(6) . ?
Re1 C4 1.887(10) . ?
S1 C16 1.726(8) . ?
S1 C20 1.759(7) . ?
C2 O3 1.133(12) . ?
N2 C6 1.353(12) . ?
N2 C7 1.460(12) . ?
O2 C10 1.218(10) . ?
C3 O4 1.146(11) . ?
N3 C9 1.503(11) . ?
N3 C11 1.501(11) . ?
N3 C12 1.499(10) . ?
C4 O5 1.175(12) . ?
N4 C13 1.335(12) . ?
N4 C14 1.429(10) . ?
C5 C6 1.339(14) . ?
N5 C17 1.378(11) . ?
N5 C20 1.292(11) . ?
N6 C24 1.375(11) . ?
N6 C27 1.434(13) . ?
N6 C28 1.444(11) . ?
O6 C13 1.214(11) . ?
C8 C9 1.513(13) . ?
C10 C11 1.523(12) . ?
C12 C13 1.542(11) . ?
C14 C15 1.382(12) . ?
C14 C19 1.407(12) . ?
C15 C16 1.394(12) . ?
C16 C17 1.408(11) . ?
C17 C18 1.398(12) . ?
C18 C19 1.383(12) . ?
C20 C21 1.474(11) . ?
C21 C22 1.378(12) . ?
C21 C26 1.400(11) . ?
C22 C23 1.372(12) . ?
C23 C24 1.411(12) . ?
C24 C25 1.407(12) . ?
C25 C26 1.370(13) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6196(12)
2 0.3804(12)
