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_7116766
_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         'C37 H51 F3 Mn N7 O3 S, C F3 O3 S, C4 H8 O'
_chemical_formula_sum            'C42 H59 F6 Mn N7 O7 S2'
_chemical_formula_weight         1007.02
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-10-24 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6932(11)
_cell_length_b                   16.2784(17)
_cell_length_c                   27.670(3)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.39
_cell_volume                     4816.5(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      171(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm90c
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10636
_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         27.126
_diffrn_reflns_theta_min         1.451
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.8651
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2108
_exptl_crystal_id                cm90c
_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, 4, 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.538
_exptl_crystal_size_mid          0.495
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 4369 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10636
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0382P)^2^+0.9507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10080
_reflns_number_total             10636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08603a2.cif
_cod_data_source_block           cm90cas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_cell_volume        4816.4(9)
_cod_original_sg_symbol_H-M      'P2(1)2(1)2(1) '
_cod_database_code               7116766
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.837
_shelxl_version_number           2014-3
_shelx_res_checksum              31585