New structural motifs in Mn cluster chemistry from the ketone/gem-diol and bis(gem¬-diol) forms of 2,6-di-(2-pyridylcarbonyl)pyridine: {MnII4MnIII2} and {MnII4MnIII6} complexes
Giannopoulos, Dimosthenis; Cunha-Silva, Luis; Ballesteros-Garrido, Rafael; Ballesteros, Rafael; Abarca, Belén; Escuer, Albert; Stamatatos, Theocharis; RSC Adv.  (2016) –; doi:10.1039/C6RA22953K

data_7226968
_publ_section_title
;
 New structural motifs in Mn cluster chemistry from the ketone/gem-diol
 and bis(gem&#x00AC;-diol) forms of 2,6-di-(2-pyridylcarbonyl)pyridine:
 {MnII4MnIII2} and {MnII4MnIII6} complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA22953K
_journal_year                    2016
_chemical_formula_moiety         'C86 H88 Mn10 N54 O22, 2(C3 H7 N O), C2 H3 N'
_chemical_formula_sum            'C94 H105 Mn10 N57 O24'
_chemical_formula_weight         2966.74
_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_date             '29 July 2016'
_audit_creation_method           'SHELXL-2014/7 and enCIFer'
_audit_update_record
;
2016-10-19 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.953(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.294(6)
_cell_length_b                   28.311(6)
_cell_length_c                   16.462(3)
_cell_measurement_reflns_used    9739
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      2.50
_cell_volume                     13404(5)
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            163590
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        23.323
_diffrn_reflns_theta_max         23.323
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'SADABS V2012/1 (Bruker AXS Inc.)' 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             6040
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1584
_refine_ls_number_reflns         19153
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.0978
_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^)+(0.1080P)^2^+310.4599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12277
_reflns_number_total             19153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra22953k1.cif
_cod_data_source_block           dg549c_sq
_cod_database_code               7226968
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              45636
_shelx_fab_checksum              30664