#------------------------------------------------------------------------------
#$Date: 2021-01-07 08:24:15 +0200 (Thu, 07 Jan 2021) $
#$Revision: 260769 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/60/7706013.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_7706013
loop_
_publ_author_name
'Arata, Shogo'
'Suzuki, Kosuke'
'Yamaguchi, Kazuya'
'Sunada, Yusuke'
_publ_section_title
;
 Supersilyl as an effective monodentate ligand to stabilize
 four-coordinate manganese(II) complexes.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17537
_journal_page_last               17541
_journal_paper_doi               10.1039/d0dt03837g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C26 H70 Br2 Mn2 O2 Si8'
_chemical_formula_sum            'C26 H70 Br2 Mn2 O2 Si8'
_chemical_formula_weight         909.21
_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_update_record
;
2020-08-31 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.848(4)
_cell_angle_beta                 107.188(5)
_cell_angle_gamma                96.065(5)
_cell_formula_units_Z            1
_cell_length_a                   9.482(4)
_cell_length_b                   10.595(4)
_cell_length_c                   13.023(5)
_cell_measurement_reflns_used    3164
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.14
_cell_volume                     1241.4(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2017/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16571
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         3.144
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             474.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0396P)²+0.7005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4885
_reflns_number_total             5517
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d0dt03837g2.cif
_cod_data_source_block           '[(Si)(THF)Mn(m-Br]2'
_cod_depositor_comments
'Adding full bibliography for 7706013--7706016.cif.'
_cod_database_code               7706013
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -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
Br1 Br 0.34727(3) 0.10070(3) 0.42660(2) 0.05331(13) Uani 1 1 d . . . . .
Mn1 Mn 0.60006(5) 0.13430(4) 0.57317(3) 0.03840(13) Uani 1 1 d . . . . .
Si1 Si 0.63421(8) 0.25071(6) 0.75058(5) 0.03432(16) Uani 1 1 d . . . . .
Si2 Si 0.40014(9) 0.26902(8) 0.76981(7) 0.0464(2) Uani 1 1 d . . . . .
Si3 Si 0.76674(10) 0.13450(9) 0.89020(7) 0.0520(2) Uani 1 1 d . . . . .
Si4 Si 0.75857(10) 0.45538(8) 0.76239(7) 0.0491(2) Uani 1 1 d . . . . .
O1 O 0.7368(3) 0.1991(3) 0.47801(19) 0.0634(6) Uani 1 1 d . . . . .
C1 C 0.4034(5) 0.3192(5) 0.9089(4) 0.0818(13) Uani 1 1 d . . . . .
H1A H 0.465683 0.399516 0.930624 0.098 Uiso 1 1 calc R U . . .
H1B H 0.303227 0.328926 0.909753 0.098 Uiso 1 1 calc R U . . .
H1C H 0.443129 0.255127 0.958331 0.098 Uiso 1 1 calc R U . . .
C2 C 0.3067(5) 0.3874(5) 0.6747(4) 0.0875(14) Uani 1 1 d . . . . .
H2A H 0.303879 0.362997 0.601977 0.105 Uiso 1 1 calc R U . . .
H2B H 0.206121 0.389369 0.678084 0.105 Uiso 1 1 calc R U . . .
H2C H 0.361834 0.470990 0.694914 0.105 Uiso 1 1 calc R U . . .
C3 C 0.2786(5) 0.1142(4) 0.7335(4) 0.0746(11) Uani 1 1 d . . . . .
H3A H 0.274087 0.084953 0.661504 0.089 Uiso 1 1 calc R U . . .
H3B H 0.319225 0.051708 0.784312 0.089 Uiso 1 1 calc R U . . .
H3C H 0.179323 0.125506 0.735733 0.089 Uiso 1 1 calc R U . . .
C4 C 0.6563(5) -0.0185(4) 0.8997(4) 0.0807(12) Uani 1 1 d . . . . .
H4A H 0.626761 -0.065704 0.830861 0.097 Uiso 1 1 calc R U . . .
H4B H 0.716227 -0.068070 0.954440 0.097 Uiso 1 1 calc R U . . .
H4C H 0.568454 -0.001566 0.918788 0.097 Uiso 1 1 calc R U . . .
C5 C 0.8199(7) 0.2203(6) 1.0249(3) 0.1001(16) Uani 1 1 d . . . . .
H5A H 0.877811 0.300788 1.022815 0.120 Uiso 1 1 calc R U . . .
H5B H 0.730839 0.235499 1.043072 0.120 Uiso 1 1 calc R U . . .
H5C H 0.878612 0.168995 1.078723 0.120 Uiso 1 1 calc R U . . .
C6 C 0.9393(5) 0.0948(5) 0.8610(4) 0.0893(14) Uani 1 1 d . . . . .
H6A H 0.999845 0.172639 0.855506 0.107 Uiso 1 1 calc R U . . .
H6B H 0.995153 0.046478 0.918764 0.107 Uiso 1 1 calc R U . . .
H6C H 0.912385 0.044680 0.793709 0.107 Uiso 1 1 calc R U . . .
C7 C 0.7256(7) 0.5650(4) 0.8647(4) 0.0980(17) Uani 1 1 d . . . . .
H7A H 0.755658 0.529152 0.934966 0.118 Uiso 1 1 calc R U . . .
H7B H 0.783198 0.646832 0.866907 0.118 Uiso 1 1 calc R U . . .
H7C H 0.620804 0.575868 0.845435 0.118 Uiso 1 1 calc R U . . .
C8 C 0.9647(5) 0.4508(5) 0.7977(4) 0.0871(14) Uani 1 1 d . . . . .
H8A H 0.986280 0.394677 0.746135 0.105 Uiso 1 1 calc R U . . .
H8B H 1.013273 0.535703 0.795792 0.105 Uiso 1 1 calc R U . . .
H8C H 1.001191 0.419746 0.869310 0.105 Uiso 1 1 calc R U . . .
C9 C 0.6991(6) 0.5284(4) 0.6286(4) 0.0874(14) Uani 1 1 d . . . . .
H9A H 0.715105 0.473184 0.574049 0.105 Uiso 1 1 calc R U . . .
H9B H 0.594405 0.539444 0.610506 0.105 Uiso 1 1 calc R U . . .
H9C H 0.756798 0.610408 0.631978 0.105 Uiso 1 1 calc R U . . .
C10 C 0.8960(5) 0.1949(7) 0.5148(5) 0.118(2) Uani 1 1 d . . . . .
H10A H 0.941540 0.247887 0.581095 0.141 Uiso 1 1 calc R U . . .
H10B H 0.919193 0.107567 0.528561 0.141 Uiso 1 1 calc R U . . .
C11 C 0.9488(8) 0.2434(13) 0.4286(7) 0.212(6) Uani 1 1 d . . . . .
H11A H 1.013757 0.322983 0.453458 0.255 Uiso 1 1 calc R U . . .
H11B H 1.007277 0.182214 0.407811 0.255 Uiso 1 1 calc R U . . .
C12 C 0.8318(9) 0.2650(7) 0.3399(6) 0.133(3) Uani 1 1 d . . . . .
H12A H 0.828843 0.209169 0.278498 0.160 Uiso 1 1 calc R U . . .
H12B H 0.843284 0.353402 0.319845 0.160 Uiso 1 1 calc R U . . .
C13 C 0.6929(6) 0.2379(5) 0.3707(4) 0.0898(14) Uani 1 1 d . . . . .
H13A H 0.641647 0.314192 0.365999 0.108 Uiso 1 1 calc R U . . .
H13B H 0.625830 0.170368 0.322945 0.108 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Mn Mn 0.3368 0.7283
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Br Br -0.2901 2.4595
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(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
Mn1 Br1 Mn1 83.840(18) . 2_656 ?
O1 Mn1 Si1 118.65(7) . . ?
O1 Mn1 Br1 99.51(8) . . ?
Si1 Mn1 Br1 122.00(3) . . ?
O1 Mn1 Br1 96.54(8) . 2_656 ?
Si1 Mn1 Br1 118.72(3) . 2_656 ?
Br1 Mn1 Br1 96.161(18) . 2_656 ?
Si3 Si1 Si2 109.18(4) . . ?
Si3 Si1 Si4 109.16(5) . . ?
Si2 Si1 Si4 107.82(4) . . ?
Si3 Si1 Mn1 109.31(4) . . ?
Si2 Si1 Mn1 108.46(4) . . ?
Si4 Si1 Mn1 112.85(4) . . ?
C1 Si2 C3 107.1(2) . . ?
C1 Si2 C2 108.2(2) . . ?
C3 Si2 C2 106.9(2) . . ?
C1 Si2 Si1 114.21(15) . . ?
C3 Si2 Si1 110.70(14) . . ?
C2 Si2 Si1 109.52(14) . . ?
C4 Si3 C5 107.3(3) . . ?
C4 Si3 C6 107.2(2) . . ?
C5 Si3 C6 108.9(3) . . ?
C4 Si3 Si1 110.88(15) . . ?
C5 Si3 Si1 113.45(18) . . ?
C6 Si3 Si1 108.94(14) . . ?
C7 Si4 C9 107.9(3) . . ?
C7 Si4 C8 107.1(2) . . ?
C9 Si4 C8 107.0(2) . . ?
C7 Si4 Si1 114.11(15) . . ?
C9 Si4 Si1 109.56(15) . . ?
C8 Si4 Si1 110.91(16) . . ?
C13 O1 C10 110.1(3) . . ?
C13 O1 Mn1 128.2(3) . . ?
C10 O1 Mn1 121.3(3) . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si3 C4 H4A 109.5 . . ?
Si3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si3 C5 H5A 109.5 . . ?
Si3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si3 C6 H6A 109.5 . . ?
Si3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si4 C7 H7A 109.5 . . ?
Si4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si4 C8 H8A 109.5 . . ?
Si4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si4 C9 H9A 109.5 . . ?
Si4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 O1 105.0(5) . . ?
C11 C10 H10A 110.7 . . ?
O1 C10 H10A 110.7 . . ?
C11 C10 H10B 110.7 . . ?
O1 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
C12 C11 C10 111.3(5) . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 107.1(5) . . ?
C11 C12 H12A 110.3 . . ?
C13 C12 H12A 110.3 . . ?
C11 C12 H12B 110.3 . . ?
C13 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
O1 C13 C12 106.2(5) . . ?
O1 C13 H13A 110.5 . . ?
C12 C13 H13A 110.5 . . ?
O1 C13 H13B 110.5 . . ?
C12 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
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
Br1 Mn1 2.5711(9) . ?
Br1 Mn1 2.5905(10) 2_656 ?
Mn1 O1 2.116(2) . ?
Mn1 Si1 2.5205(11) . ?
Si1 Si3 2.3332(12) . ?
Si1 Si2 2.3332(14) . ?
Si1 Si4 2.3366(12) . ?
Si2 C1 1.870(4) . ?
Si2 C3 1.871(4) . ?
Si2 C2 1.877(4) . ?
Si3 C4 1.861(4) . ?
Si3 C5 1.868(4) . ?
Si3 C6 1.873(4) . ?
Si4 C7 1.871(4) . ?
Si4 C9 1.872(5) . ?
Si4 C8 1.877(5) . ?
O1 C13 1.416(5) . ?
O1 C10 1.448(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.439(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.386(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.487(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 O1 C10 C11 4.8(8) . . . . ?
Mn1 O1 C10 C11 178.7(6) . . . . ?
O1 C10 C11 C12 -5.4(12) . . . . ?
C10 C11 C12 C13 4.0(13) . . . . ?
C10 O1 C13 C12 -2.6(6) . . . . ?
Mn1 O1 C13 C12 -175.9(4) . . . . ?
C11 C12 C13 O1 -0.8(9) . . . . ?
