Azide groups in high oxidation state Mn carboxylate chemistry: a new Mn(11) complex and its conversion to a Mn(25) azide complex with Me(3)SiN(3).
Stamatatos, Theocharis C; Vinslava, Alina; Abboud, Khalil A; Christou, George; Chemical communications (Cambridge, England) 34 (2009) 2839–2841; doi:10.1039/b902016k

data_7104440
_publ_section_title
;
 Azide groups in high oxidation state Mn carboxylate chemistry: a new
 Mn(11) complex and its conversion to a Mn(25) azide complex with
 Me(3)SiN(3).
;
_journal_issue                   20
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2839
_journal_page_last               2841
_journal_paper_doi               10.1039/b902016k
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C105 H75 Mn11 O42, 2(C H3 N O2), C7 H6 O2'
_chemical_formula_sum            'C105 H75 Mn11 O42'
_chemical_formula_weight         2612.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-03-04 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.655(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.247(3)
_cell_length_b                   26.842(3)
_cell_length_c                   31.920(4)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     23414(5)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1344
_diffrn_reflns_av_sigmaI/netI    0.1622
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            105514
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.9413
_exptl_absorpt_correction_T_min  0.8473
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             10528
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The asymmetric unit consists of two Mn11 clusters, two benzoic acid solvent
molecules and four nitromethane solvent molecules. All solvent molecules were
disordered and could not be modeled properly, thus program SQUEEZE, a part of
the PLATON package of crystallographic software, was used to calculate the
solvent disorder area and remove its contribution to the overall intensity
data. The crystal was very small and the crystals were solvent sensitive. Thus
the refinement did not provide for a refined model without restraints. The
phenyl rings at Carbon atoms C31, C51, C111, C171, C251, C261 were all refined
with equivalent displacements parameters using subroutine ?EADP? in the SHELXTL
refinement. Additionally, phenyl rings at Carbon atoms C31, C51, C552, C61,
C71, C81, C111, C121, C171, C221, C231, C241, C251, C261, C291, were idealized
to be equivalent to an ideal hexagon and treated as a rigid groups.
;
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2419
_refine_ls_number_reflns         30616
_refine_ls_number_restraints     1767
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                12502
_reflns_number_total             30616
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b902016k.txt
_cod_data_source_block           st342
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7104440