Structurally characterized terminal manganese(iv) oxo tris(alkoxide) complex.
Halbach, Robert L.; Gygi, David; Bloch, Eric D.; Anderson, Bryce L.; Nocera, Daniel G.; Chemical science 9 (2018) 4524–4528; doi:10.1039/c8sc01164h

data_1549312
_publ_section_title
;
 Structurally characterized terminal manganese(iv) oxo tris(alkoxide)
 complex.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              4524
_journal_page_last               4528
_journal_paper_doi               10.1039/c8sc01164h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C38 H79 K Mn O5'
_chemical_formula_sum            'C38 H79 K Mn O5'
_chemical_formula_weight         710.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-12 deposited with the CCDC.
2018-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.0930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3234(12)
_cell_length_b                   15.9361(10)
_cell_length_c                   16.7710(11)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.847
_cell_measurement_theta_min      2.556
_cell_volume                     4148.8(5)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36865
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8188.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.424
_exptl_crystal_size_min          0.422
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4972
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0517
_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/[\s^2^(Fo^2^)+(0.0693P)^2^+7.9685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4277
_reflns_number_total             4972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01164h2.cif
_cod_data_source_block           cmpd_1_mn(ditox)3k(thf)2
_cod_depositor_comments
'Adding full bibliography for 1549310--1549312.cif.'
_cod_database_code               1549312
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.756
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) =
Uanis(C16A) = Uanis(C17A) = Uanis(C18A) = Uanis(C19A) = Uanis(C20A) =
Uanis(C11B) = Uanis(C12B) = Uanis(C13B) = Uanis(C14B) = Uanis(C15B) =
Uanis(C16B) = Uanis(C17B) = Uanis(C18B) = Uanis(C19B) = Uanis(C20B)
Uanis(C31A) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A) = Uanis(C31B) =
Uanis(C32B) = Uanis(C33B) = Uanis(C34B)
3. Same fragment restrains
{C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A} sigma for 1-2:
0.02, 1-3: 0.04
{C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B} sigma for 1-2:
0.02, 1-3: 0.04
as
{C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A}
{O3A, C31A, C32A, C33A, C34A} sigma for 1-2: 0.02, 1-3: 0.04
{O3B, C31B, C32B, C33B, C34B} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3A, C31A, C32A, C33A, C34A}
4. Others
 Sof(O3B)=Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(C11B)=Sof(C12B)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=
 Sof(C16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20B)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=0.5*(1-FVAR(2))
 Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14A)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20A)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=0.5*FVAR(2)
 Sof(O3A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=FVAR(1)
 Fixed Sof: O2A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B), C34A(H34A,H34B), C31B(H31C,
 H31D), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,H34D)
5.b Me refined with riding coordinates and stretchable bonds:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13A(H13A,H13B,H13C),
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C17A(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,H20E,H20F)
;
_shelx_res_checksum              16081
_olex2_submission_special_instructions 'No special instructions were received'