#------------------------------------------------------------------------------
#$Date: 2024-05-05 04:59:37 +0300 (Sun, 05 May 2024) $
#$Revision: 291585 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/11/1571146.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_1571146
loop_
_publ_author_name
'Pérez-Bitrián, Alberto'
'Munárriz, Julen'
'Krause, Konstantin B.'
'Schlögl, Johanna'
'Hoffmann, Kurt F.'
'Sturm, Johanna S.'
'Hadi, Amiera N.'
'Teutloff, Christian'
'Wiesner, Anja'
'Limberg, Christian'
'Riedel, Sebastian'
_publ_section_title
;
 Questing for homoleptic mononuclear manganese complexes with monodentate
 O-donor ligands.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5564
_journal_page_last               5572
_journal_paper_doi               10.1039/d4sc00543k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'F20 Mn O4 Te4, 2(C24 H20 P)'
_chemical_formula_sum            'C48 H40 F20 Mn O4 P2 Te4'
_chemical_formula_weight         1688.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-08 deposited with the CCDC.	2024-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8607(3)
_cell_length_b                   11.8607(3)
_cell_length_c                   39.8339(19)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    130.00
_cell_measurement_theta_max      26.357
_cell_measurement_theta_min      2.303
_cell_volume                     5603.7(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130.00
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            49322
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_min         2.302
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_T_max  0.9047
_exptl_absorpt_correction_T_min  0.7212
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1415 before and 0.0857 after correction.
The Ratio of minimum to maximum transmission is 0.7972.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_description       block
_exptl_crystal_F_000             3212
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0299
_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)+(0.0174P)²+33.7590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2391
_reflns_number_total             2771
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc00543k2.cif
_cod_data_source_block           run_absorp_a
_cod_depositor_comments          'Adding full bibliography for 1571146.cif.'
_cod_original_cell_volume        5603.7(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1571146
_shelx_shelxl_version_number     2019/1
_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   0.816
_shelx_estimated_absorpt_t_min   0.676
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C12(H12), C9(H9), C2(H2), C8(H8), C6(H6), C5(H5), C3(H3),
 C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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
Te1 Te 0.25951(2) 0.74930(2) 0.33397(2) 0.02816(9) Uani 1 1 d . . . . .
Mn1 Mn 0.000000 0.750000 0.375000 0.0331(3) Uani 1 4 d S T P . .
P1 P 0.500000 0.250000 0.28466(3) 0.0181(2) Uani 1 2 d S T P . .
F4 F 0.2365(3) 0.7551(3) 0.28848(6) 0.0543(7) Uani 1 1 d . . . . .
F2 F 0.3058(3) 0.7366(2) 0.37814(7) 0.0577(8) Uani 1 1 d . . . . .
F3 F 0.2169(3) 0.6000(2) 0.33492(8) 0.0603(8) Uani 1 1 d . . . . .
F5 F 0.3259(3) 0.8891(2) 0.33114(8) 0.0658(9) Uani 1 1 d . . . . .
O1 O 0.1241(3) 0.8013(3) 0.34380(8) 0.0519(9) Uani 1 1 d . . . . .
C7 C 0.4947(3) 0.1270(3) 0.25841(8) 0.0216(7) Uani 1 1 d . . . . .
F1 F 0.3986(3) 0.6931(4) 0.32402(11) 0.0939(13) Uani 1 1 d . . . . .
C10 C 0.5004(4) -0.0648(3) 0.21889(10) 0.0344(9) Uani 1 1 d . . . . .
H10 H 0.502239 -0.131143 0.205529 0.041 Uiso 1 1 calc R U . . .
C4 C 0.1901(3) 0.2559(3) 0.35247(10) 0.0292(8) Uani 1 1 d . . . . .
H4 H 0.124969 0.255347 0.366333 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4234(3) 0.0379(3) 0.26557(10) 0.0314(8) Uani 1 1 d . . . . .
H12 H 0.372641 0.042185 0.283985 0.038 Uiso 1 1 calc R U . . .
C1 C 0.3784(3) 0.2560(3) 0.31119(8) 0.0210(7) Uani 1 1 d . . . . .
C9 C 0.5715(3) 0.0243(3) 0.21156(10) 0.0311(8) Uani 1 1 d . . . . .
H9 H 0.622066 0.019239 0.193121 0.037 Uiso 1 1 calc R U . . .
C2 C 0.2950(3) 0.3379(3) 0.30689(10) 0.0262(7) Uani 1 1 d . . . . .
H2 H 0.302099 0.393332 0.289810 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5690(3) 0.1209(3) 0.23109(9) 0.0290(8) Uani 1 1 d . . . . .
H8 H 0.617208 0.182578 0.226017 0.035 Uiso 1 1 calc R U . . .
C6 C 0.3675(3) 0.1751(3) 0.33676(9) 0.0250(7) Uani 1 1 d . . . . .
H6 H 0.424996 0.120477 0.340107 0.030 Uiso 1 1 calc R U . . .
C5 C 0.2727(3) 0.1752(3) 0.35708(9) 0.0296(8) Uani 1 1 d . . . . .
H5 H 0.264436 0.119880 0.374144 0.036 Uiso 1 1 calc R U . . .
C3 C 0.2013(3) 0.3373(3) 0.32795(10) 0.0294(8) Uani 1 1 d . . . . .
H3 H 0.144639 0.393297 0.325419 0.035 Uiso 1 1 calc R U . . .
C11 C 0.4267(4) -0.0574(4) 0.24563(11) 0.0413(10) Uani 1 1 d . . . . .
H11 H 0.377544 -0.118637 0.250384 0.050 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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -2.00 3.00 0.0530
-2.50 0.50 -4.00 0.0240
-1.50 -0.50 -6.00 0.0150
0.00 -2.00 -4.00 0.0150
0.50 -1.50 5.00 0.0640
0.50 -1.50 7.00 0.0690
-1.50 0.50 5.00 0.0810
0.00 1.00 -3.00 0.0330
0.00 1.00 5.00 0.0700
0.50 1.50 -4.00 0.0500
3.50 -0.50 5.00 0.0900
2.50 0.50 1.00 0.0850
2.00 2.00 2.00 0.0720
2.00 2.00 10.00 0.0420
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
F4 Te1 F2 170.90(15) . . ?
F4 Te1 F3 90.91(13) . . ?
F4 Te1 F5 88.23(13) . . ?
F3 Te1 F2 89.06(13) . . ?
F5 Te1 F2 90.26(13) . . ?
F5 Te1 F3 170.24(16) . . ?
O1 Te1 F4 94.06(14) . . ?
O1 Te1 F2 95.01(15) . . ?
O1 Te1 F3 94.70(16) . . ?
O1 Te1 F5 95.05(17) . . ?
O1 Te1 F1 178.99(17) . . ?
F1 Te1 F4 86.19(17) . . ?
F1 Te1 F2 84.75(18) . . ?
F1 Te1 F3 84.32(17) . . ?
F1 Te1 F5 85.93(18) . . ?
O1 Mn1 O1 112.23(11) 16_666 . ?
O1 Mn1 O1 112.23(11) 6_464 11_566 ?
O1 Mn1 O1 112.23(11) 6_464 16_666 ?
O1 Mn1 O1 104.1(2) 6_464 . ?
O1 Mn1 O1 104.1(2) 16_666 11_566 ?
O1 Mn1 O1 112.23(11) 11_566 . ?
C7 P1 C7 108.8(2) . 6_554 ?
C1 P1 C7 109.84(15) . 6_554 ?
C1 P1 C7 110.39(15) . . ?
C1 P1 C7 109.84(15) 6_554 . ?
C1 P1 C7 110.39(15) 6_554 6_554 ?
C1 P1 C1 107.6(2) 6_554 . ?
Te1 O1 Mn1 133.97(17) . . ?
C12 C7 P1 121.4(3) . . ?
C12 C7 C8 120.3(3) . . ?
C8 C7 P1 118.2(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C11 C10 C9 120.0(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.7(3) . . ?
C7 C12 H12 120.4 . . ?
C11 C12 C7 119.3(4) . . ?
C11 C12 H12 120.4 . . ?
C2 C1 P1 121.8(3) . . ?
C2 C1 C6 119.9(3) . . ?
C6 C1 P1 118.3(3) . . ?
C10 C9 H9 120.0 . . ?
C10 C9 C8 120.0(3) . . ?
C8 C9 H9 120.0 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.5(3) . . ?
C9 C8 H8 120.3 . . ?
C1 C6 H6 120.1 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
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
Te1 F4 1.834(3) . ?
Te1 F2 1.849(3) . ?
Te1 F3 1.842(3) . ?
Te1 F5 1.840(3) . ?
Te1 O1 1.764(3) . ?
Te1 F1 1.823(3) . ?
Mn1 O1 2.020(3) . ?
Mn1 O1 2.020(3) 11_566 ?
Mn1 O1 2.020(3) 6_464 ?
Mn1 O1 2.020(3) 16_666 ?
P1 C7 1.796(3) . ?
P1 C7 1.796(3) 6_554 ?
P1 C1 1.789(3) 6_554 ?
P1 C1 1.789(3) . ?
C7 C12 1.384(5) . ?
C7 C8 1.402(5) . ?
C10 H10 0.9500 . ?
C10 C9 1.384(6) . ?
C10 C11 1.381(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(5) . ?
C4 C3 1.379(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.382(5) . ?
C1 C2 1.397(5) . ?
C1 C6 1.406(5) . ?
C9 H9 0.9500 . ?
C9 C8 1.386(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(5) . ?
C8 H8 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.386(5) . ?
C5 H5 0.9500 . ?
C3 H3 0.9500 . ?
C11 H11 0.9500 . ?
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
P1 C7 C12 C11 -176.6(3) . . . . ?
P1 C7 C8 C9 176.2(3) . . . . ?
P1 C1 C2 C3 178.9(3) . . . . ?
P1 C1 C6 C5 -178.0(3) . . . . ?
F4 Te1 O1 Mn1 130.0(3) . . . . ?
F2 Te1 O1 Mn1 -50.7(3) . . . . ?
F3 Te1 O1 Mn1 38.8(3) . . . . ?
F5 Te1 O1 Mn1 -141.4(3) . . . . ?
C7 P1 C7 C12 -137.3(4) 6_554 . . . ?
C7 P1 C7 C8 45.6(2) 6_554 . . . ?
C7 P1 C1 C2 9.0(3) 6_554 . . . ?
C7 P1 C1 C2 -111.0(3) . . . . ?
C7 P1 C1 C6 68.6(3) . . . . ?
C7 P1 C1 C6 -171.5(3) 6_554 . . . ?
C7 C12 C11 C10 0.3(7) . . . . ?
C10 C9 C8 C7 0.6(6) . . . . ?
C12 C7 C8 C9 -0.9(6) . . . . ?
C1 P1 C7 C12 -16.7(4) . . . . ?
C1 P1 C7 C12 101.8(3) 6_554 . . . ?
C1 P1 C7 C8 166.2(3) . . . . ?
C1 P1 C7 C8 -75.3(3) 6_554 . . . ?
C1 P1 C1 C2 129.2(3) 6_554 . . . ?
C1 P1 C1 C6 -51.3(2) 6_554 . . . ?
C1 C2 C3 C4 -0.9(6) . . . . ?
C1 C6 C5 C4 -1.0(5) . . . . ?
C9 C10 C11 C12 -0.6(7) . . . . ?
C2 C1 C6 C5 1.6(5) . . . . ?
C8 C7 C12 C11 0.4(6) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
C5 C4 C3 C2 1.5(6) . . . . ?
C3 C4 C5 C6 -0.5(6) . . . . ?
C11 C10 C9 C8 0.2(6) . . . . ?
