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_1549311
_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         'C30 H63 Mn O3, C20 H40 K O10'
_chemical_formula_sum            'C50 H103 K Mn O13'
_chemical_formula_weight         1006.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.5520(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3584(5)
_cell_length_b                   17.2479(8)
_cell_length_c                   29.1110(13)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.597
_cell_measurement_theta_min      2.240
_cell_volume                     5701.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.01
_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  0.0718
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            91839
_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         26.372
_diffrn_reflns_theta_min         1.372
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.7876.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.637
_exptl_crystal_size_min          0.51
_refine_diff_density_max         1.628
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         11671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1122P)^2^+14.2121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8039
_reflns_number_total             11671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01164h2.cif
_cod_data_source_block           mn(ditox)3k(15c5)2
_cod_depositor_comments
'Adding full bibliography for 1549310--1549312.cif.'
_cod_database_code               1549311
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.798
_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.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C31(H31A,H31B), C33(H33A,H33B), C40(H40A,H40B), C39(H39A,
 H39B), C32(H32A,H32B), C36(H36A,H36B), C42(H42A,H42B), C35(H35A,H35B),
 C43(H43A,H43B), C45(H45A,H45B), C49(H49A,H49B), C44(H44A,H44B), C34(H34A,H34B),
  C37(H37A,H37B), C47(H47A,H47B), C48(H48A,H48B), C41(H41A,H41B), C50(H50A,
 H50B), C46(H46A,H46B)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C5(H5A,H5B,H5C), C24(H24A,H24B,
 H24C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C4(H4A,H4B,H4C), C27(H27A,
 H27B,H27C), C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C),
 C19(H19A,H19B,H19C), C3(H3A,H3B,H3C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C),
  C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C23(H23A,H23B,
 H23C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              31274
_olex2_submission_special_instructions 'No special instructions were received'