Exploring Mn-O bonding in the context of an electronically flexible secondary coordination sphere: synthesis of a Mn(III)-oxo
Yun Ji Park; Ellen M. Matson; Mark J. Nilges; Alison R. Fout; Chem.Commun. 51 (2015) 5310–; doi:10.1039/C4cc08603A

data_7116764
_publ_section_title
;
 Exploring Mn-O bonding in the context of an electronically flexible
 secondary coordination sphere: synthesis of a Mn(III)-oxo
;
_journal_name_full               Chem.Commun.
_journal_page_first              5310
_journal_paper_doi               10.1039/C4cc08603A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C48 H74 K Mn N7 O4'
_chemical_formula_sum            'C48 H74 K Mn N7 O4'
_chemical_formula_weight         907.18
_chemical_name_systematic
; 
? 
;
_chemical_properties_physical
'Air-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2014-10-24 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9139(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.141(3)
_cell_length_b                   9.7932(14)
_cell_length_c                   22.661(3)
_cell_measurement_reflns_used    8055
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.27
_cell_volume                     4938.7(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      174(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  c29das
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54055
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         1.830
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.7956
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1948
_exptl_crystal_id                c29das
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     947
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0585P)^2^+4.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6725
_reflns_number_total             9058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08603a2.cif
_cod_data_source_block           c29das
_cod_original_cell_volume        4938.6(12)
_cod_database_code               7116764
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2014/6
_shelx_res_checksum              3431