HAA by the first {Mn(iii)OH} complex with all O-donor ligands.
Moore, Shawn M.; Sun, Chen; Steele, Jennifer L.; Laaker, Ellen M.; Rheingold, Arnold L.; Doerrer, Linda H.; Chemical science 14 (2023) 8187–8195; doi:10.1039/d3sc01971c

data_1569512
_publ_section_title
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 HAA by the first {Mn(iii)OH} complex with all O-donor ligands.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              8187
_journal_page_last               8195
_journal_paper_doi               10.1039/d3sc01971c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C27 H37 F24 K2 Mn O8'
_chemical_formula_sum            'C27 H37 F24 K2 Mn O8'
_chemical_formula_weight         1078.70
_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     dual
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-05 deposited with the CCDC.	2023-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                78.016(2)
_cell_angle_beta                 70.970(2)
_cell_angle_gamma                84.166(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3681(5)
_cell_length_b                   11.9761(6)
_cell_length_c                   16.7124(8)
_cell_measurement_reflns_used    9059
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      72.058
_cell_measurement_theta_min      2.846
_cell_volume                     2102.67(17)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX4 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Montel
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63123
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         5.183
_diffrn_source                   'Microfocus sealed tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.729
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.3998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1564 before and 0.1165 after correction.
The Ratio of minimum to maximum transmission is 0.5306.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       needle
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     658
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0677
_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/[\s^2^(Fo^2^)+(0.1169P)^2^+4.0924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6533
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01971c2.cif
_cod_data_source_block           smm_3_276_0m_Compound_3
_cod_depositor_comments
'Adding full bibliography for 1569508--1569512.cif.'
_cod_original_cell_volume        2102.67(18)
_cod_database_code               1569512
_publcif_datablock.id            {b53ac8c0-d35b-43de-9a87-083b675cc1c1}
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H) groups, {H20A,H20B,H20C,H20D,H20E,H20F} of C20, {H21A,H21B,H21C,
  H21D,H21E,H21F} of C21, All C(H,H,H) groups
 At 1.2 times of:
  {H27G,H27H,H27I,H27J,H27K,H27L} of C27C, {H26G,H26H,H26I,H26J,H26K,H26L} of
  C26C
2. Restrained distances
 C19A-C22A
 1.52 with sigma of 0.02
 C27C-C24C
 1.5 with sigma of 0.02
 C27C-C25C
 2.45 with sigma of 0.02
 C26C-C27C
 2.45 with sigma of 0.02
 C25C-C26C
 2.45 with sigma of 0.02
 C26C-C24C = C25C-C24C
 1.5 with sigma of 0.02
 O8B-C23B
 1.42 with sigma of 0.02
 O8B-C24B
 1.42 with sigma of 0.02
 O7B-C18B
 1.43 with sigma of 0.02
 C19A-C22B
 1.52 with sigma of 0.02
 C24B-C27B
 1.54 with sigma of 0.02
 O7B-C19A
 1.43 with sigma of 0.02
 O8C-C23C
 1.42 with sigma of 0.02
 O7A-C18A
 1.43 with sigma of 0.02
 O8C-C24C
 1.42 with sigma of 0.02
 O7A-C19A
 1.43 with sigma of 0.02
 C19A-C21
 1.52 with sigma of 0.02
 C19A-C20
 1.52 with sigma of 0.02
 C24B-C26B
 1.54 with sigma of 0.02
 C23C-C24C
 2.45 with sigma of 0.02
 C25B-C24B
 1.54 with sigma of 0.02
 C13-C14
 2.42 with sigma of 0.02
 C15-C17
 2.45 with sigma of 0.02
 H23A-F5
 2 with sigma of 0.04
 C22B-C21
 2.49 with sigma of 0.04
 C27B-C25B
 2.46 with sigma of 0.04
 C26B-C27B
 2.46 with sigma of 0.04
 C22A-C20
 2.49 with sigma of 0.04
 C22A-C21
 2.49 with sigma of 0.04
 C20-C22B
 2.49 with sigma of 0.04
 C25B-C26B
 2.46 with sigma of 0.04
 C24B-C23B
 2.41 with sigma of 0.04
 C20-C21
 2.49 with sigma of 0.04
 C24C-C26C \\sim C24C-C25C \\sim C24C-C27C
 with sigma of 0.03
 C26C-C25C \\sim C25C-C27C
 with sigma of 0.04
 C24A-C27A \\sim C24A-C25A \\sim C24A-C26A
 with sigma of 0.03
 C27A-C25A \\sim C25A-C26A
 with sigma of 0.04
 O8A-C27A \\sim O8A-C25A \\sim O8A-C26A
 with sigma of 0.04
 C24B-C27B \\sim C24B-C25B \\sim C24B-C26B
 with sigma of 0.03
 C27B-C25B \\sim C25B-C26B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C24C \\sim C26C \\sim C25C \\sim C27C: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O8A \\sim C24A \\sim C27A \\sim C25A \\sim C26A \\sim C23A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C24B \\sim C27B \\sim C25B \\sim C26B \\sim C23B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C26C) = Uanis(C25B) = Uanis(C25A)
Uanis(C24A) = Uanis(C24C) = Uanis(C24B)
Uanis(C26A) = Uanis(C23B) = Uanis(C25C)
Uanis(C23C) = Uanis(C27A) = Uanis(C26B)
Uanis(O8A) = Uanis(O8C)
Uanis(O8B) = Uanis(O8C) = Uanis(O8A)
4. Rigid body (RIGU) restrains
 C24C, C26C, C25C, C27C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8A, C24A, C27A, C25A, C26A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24B, C27B, C25B, C26B, C23B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(O8A)+Sof(C24A)+Sof(C27A)+Sof(H27A)+Sof(H27B)+Sof(H27C)+Sof(C25A)+
 Sof(H25A)+Sof(H25B)+Sof(H25C)+Sof(C26A)+Sof(H26A)+Sof(H26B)+Sof(H26C)+
 Sof(C23A)+Sof(H23A)+Sof(H23B)+Sof(H23C)]+1*[Sof(O8B)+Sof(C24B)+Sof(C27B)+
 Sof(H27D)+Sof(H27E)+Sof(H27F)+Sof(C25B)+Sof(H25D)+Sof(H25E)+Sof(H25F)+
 Sof(C26B)+Sof(H26D)+Sof(H26E)+Sof(H26F)+Sof(C23B)+Sof(H23D)+Sof(H23E)+
 Sof(H23F)]+1*[Sof(O8C)+Sof(C23C)+Sof(H23G)+Sof(H23H)+Sof(H23I)+Sof(C24C)+
 Sof(C26C)+Sof(H26G)+Sof(H26H)+Sof(H26I)+Sof(H26J)+Sof(H26K)+Sof(H26L)+
 Sof(C25C)+Sof(H25G)+Sof(H25H)+Sof(H25I)+Sof(C27C)+Sof(H27G)+Sof(H27H)+
 Sof(H27I)+Sof(H27J)+Sof(H27K)+Sof(H27L)]=1 with esd of 0.0001
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O7B)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C19B)=1-FVAR(1)
 Sof(C19A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(O7A)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(O8A)=Sof(C24A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(O8B)=Sof(C24B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C25B)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C23B)=Sof(H23D)=Sof(H23E)=Sof(H23F)=FVAR(3)
 Sof(H26G)=Sof(H26H)=Sof(H26I)=Sof(H26J)=Sof(H26K)=Sof(H26L)=Sof(H27G)=
 Sof(H27H)=Sof(H27I)=Sof(H27J)=Sof(H27K)=Sof(H27L)=0.5*FVAR(5)
 Sof(O8C)=Sof(C23C)=Sof(H23G)=Sof(H23H)=Sof(H23I)=Sof(C24C)=Sof(C26C)=
 Sof(C25C)=Sof(H25G)=Sof(H25H)=Sof(H25I)=Sof(C27C)=FVAR(4)
6.a Free rotating group:
 O8A(C24A,C27A,C25A,C26A,C23A)
6.b Disordered Me refined with riding coordinates:
 C26C(H26G,H26H,H26I,H26J,H26K,H26L), C27C(H27G,H27H,H27I,H27J,H27K,H27L)
6.c Idealised Me refined as rotating group:
 C18B(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C20(H20D,H20E,H20F),
 C18A(H18D,H18E,H18F), C21(H21A,H21B,H21C), C21(H21D,H21E,H21F), C22A(H22A,H22B,
 H22C), C22B(H22D,H22E,H22F), C27A(H27A,H27B,H27C), C25A(H25A,H25B,H25C),
 C26A(H26A,H26B,H26C), C23A(H23A,H23B,H23C), C27B(H27D,H27E,H27F), C25B(H25D,
 H25E,H25F), C26B(H26D,H26E,H26F), C23B(H23D,H23E,H23F), C23C(H23G,H23H,H23I),
 C25C(H25G,H25H,H25I)
;
_shelx_res_checksum              38063
_shelx_hkl_checksum              36107
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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