Regulating the Basicity of Metal-Oxido Complexes with a Single Hydrogen Bond and Its Effect on C-H Bond Cleavage.
Barman, Suman K.; Jones, Jason R.; Sun, Chen; Hill, Ethan A.; Ziller, Joseph W.; Borovik, A. S.; Journal of the American Chemical Society 141 (2019) 11142–11150; doi:10.1021/jacs.9b03688

data_4127426
_publ_section_title
;
 Regulating the Basicity of Metal-Oxido Complexes with a Single Hydrogen
 Bond and Its Effect on C-H Bond Cleavage.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11142
_journal_page_last               11150
_journal_paper_doi               10.1021/jacs.9b03688
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C57 H103 K4 Mn2 N17 O15'
_chemical_formula_weight         1532.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.7945(9)
_cell_angle_beta                 105.6649(8)
_cell_angle_gamma                94.1267(9)
_cell_formula_units_Z            2
_cell_length_a                   14.9408(10)
_cell_length_b                   14.9961(10)
_cell_length_c                   20.1209(13)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.47
_cell_volume                     4244.3(5)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52660
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         1.519
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.166
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         20897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1348P)^2^+9.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14060
_reflns_number_total             20897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03688_si_002.cif
_cod_data_source_block           asb503
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4127426
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.913
_exptl_absorpt_special_details
; 
Reflections not merged 
52666 Corrected reflections written to file asb503s.hkl 
Estimated minimum and maximum transmission:  0.6917  0.7458 
The ratio (0.9275) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              8762
_shelx_hkl_checksum              66853
_shelx_fab_checksum              3646