#------------------------------------------------------------------------------
#$Date: 2023-05-05 03:54:54 +0300 (Fri, 05 May 2023) $
#$Revision: 283152 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/80/1568035.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_1568035
loop_
_publ_author_name
'Antico, Emanuele'
'Leutzsch, Markus'
'Wessel, Niklas'
'Weyhermüller, Thomas'
'Werlé, Christophe'
'Leitner, Walter'
_publ_section_title
;
 Selective oxidation of silanes into silanols with water using
 [MnBr(CO)₅] as a precatalyst.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              54
_journal_page_last               60
_journal_paper_doi               10.1039/d2sc05959b
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C16 H36 Mn O6, 2(C6 Br3 Mn2 O6), 4(C4 H8 O)'
_chemical_formula_sum            'C44 H68 Br6 Mn5 O22'
_chemical_formula_weight         1703.14
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-14 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                111.740(3)
_cell_angle_beta                 101.903(3)
_cell_angle_gamma                90.098(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9650(7)
_cell_length_b                   11.6978(7)
_cell_length_c                   13.6443(9)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.029
_cell_measurement_theta_min      2.560
_cell_volume                     1584.79(18)
_computing_cell_refinement       'APEX3 v2019.11-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service V6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71687
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.881
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\mS DIAMOND'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.819
_exptl_absorpt_correction_T_max  0.5735
_exptl_absorpt_correction_T_min  0.4653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             843
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.340
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9245
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0477
_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)+(0.0822P)²+0.8353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7237
_reflns_number_total             9245
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc05959b2.cif
_cod_data_source_block           CEC0111
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-SCan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1568035--1568037.cif.

 Adding full bibliography for 1568035--1568037.cif.
;
_cod_database_code               1568035
_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   0.573
_shelx_estimated_absorpt_t_max   0.699
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
Br1 Br 0.99218(3) 0.84603(3) 0.81993(3) 0.03164(10) Uani 1 1 d . . . . .
Br2 Br 0.79352(3) 0.87865(3) 0.60419(3) 0.03011(10) Uani 1 1 d . . . . .
Br3 Br 0.70071(3) 0.68665(3) 0.71342(3) 0.02779(10) Uani 1 1 d . . . . .
Mn1 Mn 0.88924(5) 0.69263(5) 0.63372(4) 0.02677(12) Uani 1 1 d . . . . .
Mn2 Mn 0.77405(5) 0.91506(5) 0.79535(4) 0.02620(12) Uani 1 1 d . . . . .
Mn3 Mn 0.500000 0.500000 0.000000 0.02467(15) Uani 1 2 d S . P . .
O2 O 0.7583(3) 0.5169(3) 0.4210(2) 0.0441(7) Uani 1 1 d . . . . .
O4 O 1.1086(3) 0.7211(3) 0.5493(3) 0.0486(8) Uani 1 1 d . . . . .
O6 O 0.9957(3) 0.4900(3) 0.6914(3) 0.0496(8) Uani 1 1 d . . . . .
O8 O 0.5190(3) 0.9899(3) 0.7578(3) 0.0443(7) Uani 1 1 d . . . . .
O10 O 0.7589(3) 0.9328(3) 1.0128(2) 0.0411(6) Uani 1 1 d . . . . .
O12 O 0.8741(3) 1.1742(3) 0.8819(3) 0.0459(7) Uani 1 1 d . . . . .
O20 O 0.5336(3) 0.6431(2) 0.1569(2) 0.0335(6) Uani 1 1 d D . . . .
H20A H 0.596(3) 0.691(4) 0.172(4) 0.050 Uiso 1 1 d D U . . .
H20B H 0.500(5) 0.650(5) 0.208(3) 0.050 Uiso 1 1 d D U . . .
O21 O 0.5701(2) 0.3616(2) 0.0674(2) 0.0305(5) Uani 1 1 d . . . . .
O31 O 0.3098(2) 0.4640(2) 0.0122(2) 0.0316(5) Uani 1 1 d . . . . .
O41 O 0.7454(3) 0.7875(3) 0.2446(3) 0.0569(10) Uani 1 1 d . . . . .
O51 O 0.4124(3) 0.6794(3) 0.3148(2) 0.0454(7) Uani 1 1 d . . . . .
C1 C 0.8070(4) 0.5859(3) 0.5024(3) 0.0334(8) Uani 1 1 d . . . . .
C3 C 1.0224(4) 0.7107(4) 0.5821(3) 0.0362(8) Uani 1 1 d . . . . .
C5 C 0.9537(4) 0.5681(4) 0.6689(3) 0.0356(8) Uani 1 1 d . . . . .
C7 C 0.6173(4) 0.9586(3) 0.7705(3) 0.0335(8) Uani 1 1 d . . . . .
C9 C 0.7658(3) 0.9259(3) 0.9290(3) 0.0315(7) Uani 1 1 d . . . . .
C11 C 0.8356(4) 1.0735(3) 0.8477(3) 0.0337(8) Uani 1 1 d . . . . .
C22 C 0.5615(4) 0.2278(3) 0.0123(3) 0.0378(8) Uani 1 1 d . . . . .
H22A H 0.630326 0.202104 -0.025978 0.045 Uiso 1 1 calc R U . . .
H22B H 0.480562 0.197280 -0.040700 0.045 Uiso 1 1 calc R U . . .
C23 C 0.5718(4) 0.1794(4) 0.1018(4) 0.0406(9) Uani 1 1 d . . . . .
H23A H 0.489871 0.174286 0.120358 0.049 Uiso 1 1 calc R U . . .
H23B H 0.604280 0.096798 0.081247 0.049 Uiso 1 1 calc R U . . .
C24 C 0.6630(4) 0.2743(4) 0.1943(4) 0.0435(10) Uani 1 1 d . . . . .
H24A H 0.750419 0.258775 0.188403 0.052 Uiso 1 1 calc R U . . .
H24B H 0.652117 0.275072 0.264827 0.052 Uiso 1 1 calc R U . . .
C25 C 0.6286(4) 0.3943(4) 0.1811(3) 0.0397(9) Uani 1 1 d . . . . .
H25A H 0.569866 0.434751 0.227092 0.048 Uiso 1 1 calc R U . . .
H25B H 0.704372 0.451725 0.202119 0.048 Uiso 1 1 calc R U . . .
C32 C 0.2274(4) 0.5598(4) 0.0491(3) 0.0347(8) Uani 1 1 d . . . . .
H32A H 0.172552 0.572032 -0.012967 0.042 Uiso 1 1 calc R U . . .
H32B H 0.276163 0.638961 0.097553 0.042 Uiso 1 1 calc R U . . .
C33 C 0.1508(4) 0.5133(4) 0.1097(4) 0.0401(9) Uani 1 1 d . . . . .
H33A H 0.195704 0.533440 0.185644 0.048 Uiso 1 1 calc R U . . .
H33B H 0.068585 0.548257 0.108755 0.048 Uiso 1 1 calc R U . . .
C34 C 0.1362(4) 0.3751(4) 0.0455(4) 0.0426(10) Uani 1 1 d . . . . .
H34A H 0.115743 0.328960 0.088770 0.051 Uiso 1 1 calc R U . . .
H34B H 0.070622 0.352629 -0.021975 0.051 Uiso 1 1 calc R U . . .
C35 C 0.2646(4) 0.3513(4) 0.0216(4) 0.0365(8) Uani 1 1 d . . . . .
H35A H 0.321167 0.335508 0.081085 0.044 Uiso 1 1 calc R U . . .
H35B H 0.259413 0.279080 -0.046662 0.044 Uiso 1 1 calc R U . . .
C42 C 0.8499(5) 0.7308(4) 0.2858(4) 0.0525(12) Uani 1 1 d . . . . .
H42A H 0.869974 0.658558 0.226848 0.063 Uiso 1 1 calc R U . . .
H42B H 0.831169 0.703499 0.342055 0.063 Uiso 1 1 calc R U . . .
C43 C 0.9543(5) 0.8277(5) 0.3319(5) 0.0609(14) Uani 1 1 d . . . . .
H43A H 1.004688 0.821814 0.278104 0.073 Uiso 1 1 calc R U . . .
H43B H 1.009246 0.821055 0.396612 0.073 Uiso 1 1 calc R U . . .
C44 C 0.8922(5) 0.9480(5) 0.3621(5) 0.0559(12) Uani 1 1 d . . . . .
H44A H 0.880430 0.975671 0.437160 0.067 Uiso 1 1 calc R U . . .
H44B H 0.942735 1.013697 0.355201 0.067 Uiso 1 1 calc R U . . .
C45 C 0.7723(5) 0.9176(4) 0.2846(5) 0.0645(17) Uani 1 1 d . . . . .
H45A H 0.705942 0.960020 0.320192 0.077 Uiso 1 1 calc R U . . .
H45B H 0.776536 0.944280 0.224370 0.077 Uiso 1 1 calc R U . . .
C52 C 0.3529(7) 0.7918(6) 0.3528(4) 0.0723(19) Uani 1 1 d . . . . .
H52A H 0.262459 0.777710 0.318537 0.087 Uiso 1 1 calc R U . . .
H52B H 0.390481 0.856258 0.334514 0.087 Uiso 1 1 calc R U . . .
C53 C 0.3718(6) 0.8312(5) 0.4713(4) 0.0651(16) Uani 1 1 d . . . . .
H53A H 0.294619 0.861469 0.495465 0.078 Uiso 1 1 calc R U . . .
H53B H 0.440725 0.897545 0.509152 0.078 Uiso 1 1 calc R U . . .
C54 C 0.4043(6) 0.7167(6) 0.4928(4) 0.0599(14) Uani 1 1 d . . . . .
H54A H 0.458665 0.737638 0.565757 0.072 Uiso 1 1 calc R U . . .
H54B H 0.328029 0.666772 0.486537 0.072 Uiso 1 1 calc R U . . .
C55 C 0.4718(4) 0.6501(4) 0.4068(3) 0.0401(9) Uani 1 1 d . . . . .
H55A H 0.561832 0.678993 0.430071 0.048 Uiso 1 1 calc R U . . .
H55B H 0.462987 0.559907 0.388874 0.048 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
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
Mn2 Br1 Mn1 78.204(19) . . ?
Mn2 Br2 Mn1 77.570(19) . . ?
Mn1 Br3 Mn2 77.679(19) . . ?
C3 Mn1 C5 91.24(18) . . ?
C3 Mn1 C1 91.65(19) . . ?
C5 Mn1 C1 91.31(18) . . ?
C3 Mn1 Br1 91.24(14) . . ?
C5 Mn1 Br1 90.33(13) . . ?
C1 Mn1 Br1 176.65(13) . . ?
C3 Mn1 Br3 175.17(13) . . ?
C5 Mn1 Br3 92.50(13) . . ?
C1 Mn1 Br3 91.33(13) . . ?
Br1 Mn1 Br3 85.68(2) . . ?
C3 Mn1 Br2 92.83(12) . . ?
C5 Mn1 Br2 173.88(13) . . ?
C1 Mn1 Br2 93.15(12) . . ?
Br1 Mn1 Br2 85.01(2) . . ?
Br3 Mn1 Br2 83.214(19) . . ?
C3 Mn1 Mn2 124.07(13) . . ?
C5 Mn1 Mn2 122.79(12) . . ?
C1 Mn1 Mn2 125.91(12) . . ?
Br1 Mn1 Mn2 50.843(15) . . ?
Br3 Mn1 Mn2 51.162(15) . . ?
Br2 Mn1 Mn2 51.091(16) . . ?
C11 Mn2 C7 90.96(17) . . ?
C11 Mn2 C9 90.89(18) . . ?
C7 Mn2 C9 91.52(17) . . ?
C11 Mn2 Br1 90.84(12) . . ?
C7 Mn2 Br1 176.96(12) . . ?
C9 Mn2 Br1 90.91(12) . . ?
C11 Mn2 Br2 93.45(13) . . ?
C7 Mn2 Br2 92.16(13) . . ?
C9 Mn2 Br2 174.27(12) . . ?
Br1 Mn2 Br2 85.28(2) . . ?
C11 Mn2 Br3 175.52(13) . . ?
C7 Mn2 Br3 92.32(12) . . ?
C9 Mn2 Br3 92.07(11) . . ?
Br1 Mn2 Br3 85.756(19) . . ?
Br2 Mn2 Br3 83.390(19) . . ?
C11 Mn2 Mn1 124.36(13) . . ?
C7 Mn2 Mn1 126.05(12) . . ?
C9 Mn2 Mn1 122.96(12) . . ?
Br1 Mn2 Mn1 50.953(16) . . ?
Br2 Mn2 Mn1 51.339(16) . . ?
Br3 Mn2 Mn1 51.159(16) . . ?
O20 Mn3 O20 180.0 . 2_665 ?
O20 Mn3 O31 89.65(10) . . ?
O20 Mn3 O31 90.35(10) 2_665 . ?
O20 Mn3 O31 90.35(10) . 2_665 ?
O20 Mn3 O31 89.65(10) 2_665 2_665 ?
O31 Mn3 O31 180.0 . 2_665 ?
O20 Mn3 O21 88.11(10) . 2_665 ?
O20 Mn3 O21 91.89(10) 2_665 2_665 ?
O31 Mn3 O21 88.10(10) . 2_665 ?
O31 Mn3 O21 91.90(10) 2_665 2_665 ?
O20 Mn3 O21 91.89(10) . . ?
O20 Mn3 O21 88.11(10) 2_665 . ?
O31 Mn3 O21 91.90(10) . . ?
O31 Mn3 O21 88.10(10) 2_665 . ?
O21 Mn3 O21 180.0 2_665 . ?
C25 O21 C22 109.0(3) . . ?
C25 O21 Mn3 122.7(2) . . ?
C22 O21 Mn3 128.2(2) . . ?
C32 O31 C35 109.2(3) . . ?
C32 O31 Mn3 123.8(2) . . ?
C35 O31 Mn3 123.8(2) . . ?
C45 O41 C42 110.4(3) . . ?
C52 O51 C55 108.9(3) . . ?
O2 C1 Mn1 177.9(4) . . ?
O4 C3 Mn1 179.1(4) . . ?
O6 C5 Mn1 179.3(4) . . ?
O8 C7 Mn2 177.6(4) . . ?
O10 C9 Mn2 179.1(3) . . ?
O12 C11 Mn2 179.2(4) . . ?
O21 C22 C23 104.4(3) . . ?
C24 C23 C22 103.0(3) . . ?
C23 C24 C25 102.8(3) . . ?
O21 C25 C24 106.3(3) . . ?
O31 C32 C33 104.9(3) . . ?
C34 C33 C32 102.1(3) . . ?
C35 C34 C33 101.9(3) . . ?
O31 C35 C34 105.3(3) . . ?
O41 C42 C43 105.0(4) . . ?
C42 C43 C44 104.7(4) . . ?
C45 C44 C43 103.9(4) . . ?
O41 C45 C44 107.5(4) . . ?
O51 C52 C53 107.2(4) . . ?
C52 C53 C54 104.4(4) . . ?
C55 C54 C53 103.2(4) . . ?
O51 C55 C54 104.6(3) . . ?
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 Mn2 2.5222(6) . ?
Br1 Mn1 2.5262(7) . ?
Br2 Mn2 2.5371(7) . ?
Br2 Mn1 2.5460(6) . ?
Br3 Mn1 2.5385(6) . ?
Br3 Mn2 2.5386(6) . ?
Mn1 C3 1.790(4) . ?
Mn1 C5 1.798(4) . ?
Mn1 C1 1.804(4) . ?
Mn1 Mn2 3.1840(7) . ?
Mn2 C11 1.794(4) . ?
Mn2 C7 1.794(4) . ?
Mn2 C9 1.802(4) . ?
Mn3 O20 2.131(2) . ?
Mn3 O20 2.131(2) 2_665 ?
Mn3 O31 2.179(3) . ?
Mn3 O31 2.179(3) 2_665 ?
Mn3 O21 2.208(3) 2_665 ?
Mn3 O21 2.208(3) . ?
O2 C1 1.122(5) . ?
O4 C3 1.150(5) . ?
O6 C5 1.136(5) . ?
O8 C7 1.139(5) . ?
O10 C9 1.134(5) . ?
O12 C11 1.137(5) . ?
O21 C25 1.454(5) . ?
O21 C22 1.457(4) . ?
O31 C32 1.448(4) . ?
O31 C35 1.466(4) . ?
O41 C45 1.420(6) . ?
O41 C42 1.443(6) . ?
O51 C52 1.436(6) . ?
O51 C55 1.449(5) . ?
C22 C23 1.510(6) . ?
C23 C24 1.504(6) . ?
C24 C25 1.519(6) . ?
C32 C33 1.517(5) . ?
C33 C34 1.516(6) . ?
C34 C35 1.513(6) . ?
C42 C43 1.470(7) . ?
C43 C44 1.517(7) . ?
C44 C45 1.457(7) . ?
C52 C53 1.477(7) . ?
C53 C54 1.502(8) . ?
C54 C55 1.489(6) . ?
