A Reactive Manganese(IV)-Hydroxide Complex: A Missing Intermediate in Hydrogen Atom Transfer by High-Valent Metal-Oxo Porphyrinoid Compounds.
Zaragoza, Jan Paulo T.; Siegler, Maxime A.; Goldberg, David P.; Journal of the American Chemical Society 140 (2018) 4380–4390; doi:10.1021/jacs.8b00350

data_4132023
_publ_section_title
;
 A Reactive Manganese(IV)-Hydroxide Complex: A Missing Intermediate in
 Hydrogen Atom Transfer by High-Valent Metal-Oxo Porphyrinoid Compounds.
;
_journal_issue                   12
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4380
_journal_page_last               4390
_journal_paper_doi               10.1021/jacs.8b00350
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C91 H60.42 Mn0.71 N4 O0.71, 0.847(C6 H5 F)'
_chemical_formula_sum            'C96.08 H64.66 F0.85 Mn0.71 N4 O0.71'
_chemical_formula_weight         1341.65
_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-2014/7
_cell_angle_alpha                95.5849(14)
_cell_angle_beta                 104.6130(14)
_cell_angle_gamma                109.5793(18)
_cell_formula_units_Z            2
_cell_length_a                   14.1015(2)
_cell_length_b                   15.8829(3)
_cell_length_c                   21.2236(3)
_cell_measurement_reflns_used    22952
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.97
_cell_measurement_theta_min      2.99
_cell_volume                     4246.68(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55101
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.894
_diffrn_reflns_theta_min         2.195
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       'small block'
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1229
_refine_ls_number_reflns         16602
_refine_ls_number_restraints     1423
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0921P)^2^+0.8372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14583
_reflns_number_total             16602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00350_si_002.cif
_cod_data_source_block           1_OH2
_cod_original_cell_volume        4246.67(13)
_cod_database_code               4132023
_shelx_shelxl_version_number     2014/7
_oxdiff_exptl_absorpt_empirical_full_min 0.877
_oxdiff_exptl_absorpt_empirical_full_max 1.222
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              33358
_shelx_hkl_checksum              14839
_shelx_fab_checksum              74178