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_7116765
_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         'C36 H51 Mn N7 O, C4 H8 O'
_chemical_formula_structural     'C40 H59 Mn N7 O2'
_chemical_formula_sum            'C40 H59 Mn N7 O2'
_chemical_formula_weight         724.88
_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_cell_setting           monoclinic
_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
_audit_update_record
;
2014-10-24 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.193(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7762(4)
_cell_length_b                   9.2337(4)
_cell_length_c                   42.2828(18)
_cell_measurement_reflns_used    3863
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      66.67
_cell_measurement_theta_min      4.18
_cell_volume                     3816.9(3)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.964
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  cc54cas
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            6616
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.510
_diffrn_reflns_theta_min         2.090
_exptl_absorpt_coefficient_mu    3.150
_exptl_absorpt_correction_T_max  0.6891
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_id                cc54cas
_exptl_crystal_preparation
; 
The data crystal was mounted using Paratone-N oil to a 
0.3 mm cryo-loop (Hampton Research) with the (-1, 2, -2) 
scattering planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0545P)^2^+0.8801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5758
_reflns_number_total             6616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08603a2.cif
_cod_data_source_block           cc54cas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7116765
_shelx_estimated_absorpt_t_min   0.463
_shelx_estimated_absorpt_t_max   0.633
_shelxl_version_number           2014-3
_shelx_res_checksum              50206