#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:17:55 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/06/7700620.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_7700620
loop_
_publ_author_name
'Gayfulin, Yakov M.'
'Brylev, Konstantin A.'
'Ryzhikov, Maxim R.'
'Samsonenko, Denis G.'
'Kitamura, Noboru'
'Mironov, Yuri V.'
_publ_section_title
;
 Luminescent twelve-nuclear rhenium clusters.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12522
_journal_page_last               12530
_journal_paper_doi               10.1039/c9dt02352f
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_sum            'C41 H100 Br9 N5 Re12 S14'
_chemical_formula_weight         4065.68
_space_group_crystal_system      hexagonal
_space_group_IT_number           189
_space_group_name_Hall           'P -6 -2'
_space_group_name_H-M_alt        'P -6 2 m'
_symmetry_space_group_name_Hall  'P -6 -2'
_symmetry_space_group_name_H-M   'P -6 2 m'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-27 deposited with the CCDC.    2019-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   11.9994(7)
_cell_length_b                   11.9994(7)
_cell_length_c                   17.3402(15)
_cell_measurement_reflns_used    1075
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      3.90
_cell_volume                     2162.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4210
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    21.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.122
_exptl_crystal_description       rod
_exptl_crystal_F_000             1820
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.25(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                992
_reflns_number_total             1463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02352f2.cif
_cod_data_source_block           gy1129-1_sq
_cod_depositor_comments
'Adding full bibliography for 7700619--7700620.cif.'
_cod_database_code               7700620
_shelx_shelxl_version_number     2018/3
_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_min   0.089
_shelx_estimated_absorpt_t_max   0.416
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z'
'x-y, -y, z'
'-x, -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
Re1 Re 0.87596(6) 0.87596(6) 0.78585(4) 0.0855(3) Uani 1 2 d S T P
Re2 Re 0.87764(6) 1.000000 0.90821(4) 0.0779(3) Uani 1 2 d S T P
S1 S 1.000000 1.000000 0.6778(4) 0.090(3) Uani 1 6 d S T P
S2 S 0.7714(5) 1.000000 0.7911(2) 0.111(2) Uani 1 2 d S T P
S3 S 0.7703(4) 0.7703(4) 0.9031(2) 0.1028(17) Uani 1 2 d S T P
Br1 Br 0.7060(2) 1.000000 1.000000 0.1395(15) Uani 1 4 d S T P
Br2 Br 0.7008(2) 0.7008(2) 0.70129(13) 0.1546(12) Uani 1 2 d S T P
C1 C 1.000000 1.000000 1.000000 0.074(12) Uani 1 12 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
Re1 Re1 Re1 60.0 3_675 2_765
Re1 Re1 Re2 60.102(17) 2_765 2_765
Re1 Re1 Re2 60.103(17) 3_675 .
Re1 Re1 Re2 89.61(2) 3_675 2_765
Re1 Re1 Re2 89.62(2) 2_765 .
Re2 Re1 Re2 58.91(3) 2_765 .
S1 Re1 Re1 57.40(9) . 2_765
S1 Re1 Re1 57.40(9) . 3_675
S1 Re1 Re2 117.44(10) . 2_765
S1 Re1 Re2 117.45(10) . .
S1 Re1 S3 173.47(15) . .
S1 Re1 Br2 93.57(12) . .
S2 Re1 Re1 57.21(7) . 3_675
S2 Re1 Re1 57.21(7) 2_765 2_765
S2 Re1 Re1 117.16(7) . 2_765
S2 Re1 Re1 117.16(7) 2_765 3_675
S2 Re1 Re2 57.54(9) . .
S2 Re1 Re2 57.54(9) 2_765 2_765
S2 Re1 Re2 116.41(9) . 2_765
S2 Re1 Re2 116.41(9) 2_765 .
S2 Re1 S1 89.98(9) . .
S2 Re1 S1 89.98(9) 2_765 .
S2 Re1 S2 172.84(16) . 2_765
S2 Re1 S3 89.62(10) . .
S2 Re1 S3 89.62(10) 2_765 .
S2 Re1 Br2 93.57(8) . .
S2 Re1 Br2 93.57(8) 2_765 .
S3 Re1 Re1 117.27(9) . 2_765
S3 Re1 Re1 117.27(9) . 3_675
S3 Re1 Re2 57.18(9) . .
S3 Re1 Re2 57.18(9) . 2_765
S3 Re1 Br2 92.96(12) . .
Br2 Re1 Re1 135.26(4) . 2_765
Br2 Re1 Re1 135.26(4) . 3_675
Br2 Re1 Re2 135.12(5) . .
Br2 Re1 Re2 135.12(5) . 2_765
Re1 Re2 Re1 59.80(3) . 3_675
Re1 Re2 Re2 145.129(15) . 4_557
Re1 Re2 Re2 145.130(15) 3_675 4_557
Re1 Re2 Br1 136.33(4) . .
Re1 Re2 Br1 136.33(4) 3_675 .
Re2 Re2 Re1 60.545(17) 2_765 .
Re2 Re2 Re1 60.545(17) 3_675 3_675
Re2 Re2 Re1 90.38(2) 2_765 3_675
Re2 Re2 Re1 90.38(2) 3_675 .
Re2 Re2 Re2 60.0 3_675 2_765
Re2 Re2 Re2 90.0 2_765 4_557
Re2 Re2 Re2 90.0 3_675 4_557
Re2 Re2 Br1 133.25(3) 2_765 .
Re2 Re2 Br1 133.25(3) 3_675 .
S2 Re2 Re1 56.91(10) . .
S2 Re2 Re1 56.91(11) . 3_675
S2 Re2 Re2 117.42(11) . 2_765
S2 Re2 Re2 117.42(11) . 3_675
S2 Re2 Re2 147.88(13) . 4_557
S2 Re2 Br1 95.58(14) . .
S3 Re2 Re1 57.41(10) . .
S3 Re2 Re1 57.41(10) 3_675 3_675
S3 Re2 Re1 117.18(10) . 3_675
S3 Re2 Re1 117.18(10) 3_675 .
S3 Re2 Re2 57.86(6) . 2_765
S3 Re2 Re2 57.86(6) 3_675 3_675
S3 Re2 Re2 92.12(10) . 4_557
S3 Re2 Re2 92.12(10) 3_675 4_557
S3 Re2 Re2 117.81(6) . 3_675
S3 Re2 Re2 117.81(6) 3_675 2_765
S3 Re2 S2 89.36(9) . .
S3 Re2 S2 89.36(9) 3_675 .
S3 Re2 S3 173.94(18) . 3_675
S3 Re2 Br1 93.01(8) . .
S3 Re2 Br1 93.01(8) 3_675 .
Br1 Re2 Re2 52.30(4) . 4_557
C1 Re2 Re1 114.41(3) . .
C1 Re2 Re1 114.41(3) . 3_675
C1 Re2 Re2 42.690(18) . 4_557
C1 Re2 Re2 54.043(14) . 2_765
C1 Re2 Re2 54.043(14) . 3_675
C1 Re2 S2 169.43(13) . .
C1 Re2 S3 90.09(8) . .
C1 Re2 S3 90.09(8) . 3_675
C1 Re2 Br1 94.99(5) . .
Re1 S1 Re1 65.20(18) 2_765 .
Re1 S1 Re1 65.20(18) 3_675 .
Re1 S1 Re1 65.20(18) 3_675 2_765
Re1 S2 Re1 65.58(15) . 3_675
Re1 S2 Re2 65.55(12) . .
Re1 S2 Re2 65.55(12) 3_675 .
Re2 S3 Re1 65.41(12) . .
Re2 S3 Re1 65.41(12) 2_765 .
Re2 S3 Re2 64.29(13) 2_765 .
Re2 Br1 Re2 75.40(9) . 4_557
Re2 C1 Re2 71.91(3) . 2_765
Re2 C1 Re2 71.91(3) 2_765 3_675
Re2 C1 Re2 71.91(3) 4_557 5_767
Re2 C1 Re2 71.91(3) 6_677 4_557
Re2 C1 Re2 71.91(3) 6_677 5_767
Re2 C1 Re2 71.92(3) . 3_675
Re2 C1 Re2 94.62(4) . 4_557
Re2 C1 Re2 94.62(4) 2_765 5_767
Re2 C1 Re2 94.62(4) 6_677 3_675
Re2 C1 Re2 140.367(14) . 6_677
Re2 C1 Re2 140.367(14) 3_675 4_557
Re2 C1 Re2 140.367(14) 3_675 5_767
Re2 C1 Re2 140.367(14) 6_677 2_765
Re2 C1 Re2 140.367(15) . 5_767
Re2 C1 Re2 140.367(15) 2_765 4_557
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
Re1 Re1 2.5780(12) 2_765 yes
Re1 Re1 2.5780(12) 3_675 ?
Re1 Re2 2.5859(8) . yes
Re1 Re2 2.5859(8) 2_765 ?
Re1 S1 2.393(6) . yes
Re1 S2 2.380(5) . yes
Re1 S2 2.380(5) 2_765 ?
Re1 S3 2.396(5) . yes
Re1 Br2 2.563(2) . yes
Re2 Re2 2.5431(12) 2_765 yes
Re2 Re2 2.5431(12) 3_675 ?
Re2 Re2 3.1835(14) 4_557 yes
Re2 S2 2.397(4) . yes
Re2 S3 2.390(4) . yes
Re2 S3 2.390(4) 3_675 ?
Re2 Br1 2.603(2) . yes
Re2 C1 2.1655(7) . yes
