Helicity inversion and redox chemistry of chiral manganese(ii) cubanes.
Deville, Claire; Granelli, Matteo; Downward, Alan M.; Besnard, Céline; Guenée, Laure; Williams, Alan F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12917–; doi:10.1039/c4dt01590h

data_7031892
_publ_section_title
;
 Helicity inversion and redox chemistry of chiral manganese(ii) cubanes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12917
_journal_paper_doi               10.1039/c4dt01590h
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C92 H80 Mn4 N16 O8 P2, 2(Cl O4)'
_chemical_formula_sum            'C92 H80 Cl2 Mn4 N16 O16 P2'
_chemical_formula_weight         2018.32
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.61754(11)
_cell_length_b                   21.61754(11)
_cell_length_c                   19.15394(11)
_cell_measurement_reflns_used    25704
_cell_measurement_temperature    179.95(10)
_cell_measurement_theta_max      72.5630
_cell_measurement_theta_min      3.2660
_cell_volume                     7751.78(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007). 40, 609-613'
_diffrn_ambient_temperature      179.95(10)
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9871
_diffrn_measurement_details
;
  1 omega -124.00  -97.40   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000    0.0000 38

  2 omega -123.00  -30.60   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -19.0000 -120.0000 132

  3 omega  -37.00    6.40   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000   30.0000  -90.0000 62

  4 omega   27.00   90.70   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000  -30.0000 91

  5 omega  113.00  138.90   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  111.0000 -150.0000 37

  6 omega   32.00  163.60   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716   15.0000  -60.0000 188

  7 omega   33.00   77.80   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -45.0000   60.0000 64

  8 omega -114.00  -27.20   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -38.0000  -30.0000 124

  9 omega    2.00   27.90   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   38.0000   60.0000 37

 10 omega -119.00  -85.40   0.7000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000  150.0000 48

 11 omega  -72.00  -40.50   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -46.0000  167.0000 45

 12 omega -133.00  -91.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000 -111.0000  -90.0000 60

 13 omega   31.00   88.40   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -45.0000  120.0000 82

 14 omega   70.00  165.90   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716   30.0000   90.0000 137

 15 omega  116.00  140.50   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -61.0000    0.0000 35

 16 omega   31.00  101.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -61.0000    0.0000 100

 17 omega   89.00  117.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716   77.0000  -60.0000 40

 18 omega   35.00   91.00   0.7000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000 -180.0000 80
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0512209000
_diffrn_orient_matrix_UB_12      -0.0215892000
_diffrn_orient_matrix_UB_13      -0.0627983000
_diffrn_orient_matrix_UB_21      0.0339191000
_diffrn_orient_matrix_UB_22      -0.0417420000
_diffrn_orient_matrix_UB_23      -0.0312456000
_diffrn_orient_matrix_UB_31      -0.0547627000
_diffrn_orient_matrix_UB_32      -0.0675667000
_diffrn_orient_matrix_UB_33      0.0393686000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42401
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         72.576
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.209
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.504
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             3108
_exptl_crystal_size_max          0.2041
_exptl_crystal_size_mid          0.1618
_exptl_crystal_size_min          0.1309
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
Hooft : 0.0041(9)
Flack x = -0.002(1) from 4320 selected quotients (Parsons' method)
;
_refine_ls_abs_structure_Flack   -0.005(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10157
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0594P)^2^+0.8001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9833
_reflns_number_total             10157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031638
_cod_data_source_file            c4dt01590h2.cif
_cod_data_source_block           8
_cod_original_cell_volume        7751.77(9)
_cod_database_code               7031892
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N11B-H11B
 0.88 with sigma of 0.02
 N11A-H11A
 0.88 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C2A(H2A), C2B(H2B)
3.b Secondary CH2 refined with riding coordinates:
 C12A(H12A,H12B), C12B(H12C,H12D)
3.c Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C15C(H15C), C7C(H7C), C16A(H16A), C14C(H14C), C19A(H19A),
 C16B(H16B), C17A(H17A), C9B(H9B), C11C(H11C), C5C(H5C), C8B(H8B), C19B(H19B),
 C9C(H9C), C18B(H18B), C17B(H17B), C7B(H7B), C8C(H8C), C6C(H6C), C8A(H8A),
 C13C(H13C), C6A(H6A), C6B(H6B), C7A(H7A), C9A(H9A), C12C(H12E)
3.d Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
;