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_7031893
_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         'C82 H68 Mn4 N18 O12, 2(Cl O4), 4(C H2 Cl2)'
_chemical_formula_sum            'C86 H76 Cl10 Mn4 N18 O20'
_chemical_formula_weight         2255.90
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-03
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.66452(13)
_cell_length_b                   17.98233(19)
_cell_length_c                   29.4766(3)
_cell_measurement_reflns_used    19222
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.5060
_cell_measurement_theta_min      3.7900
_cell_volume                     9363.22(15)
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9769
_diffrn_measurement_details
;
  1 omega -119.00  -85.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000   60.0000 68

  2 omega  -70.00   36.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   57.0000    0.0000 212

  3 omega   97.00  122.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  178.0000   60.0000 50

  4 omega -117.00  -81.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -77.0000   90.0000 72

  5 omega   41.00   80.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000   90.0000 78

  6 omega   49.00   78.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000 -180.0000 58

  7 omega   33.00   92.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -45.0000  150.0000 118

  8 omega   40.00   82.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000  -90.0000 84

  9 omega   40.00   89.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -94.0000   30.0000 98

 10 omega  111.00  164.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  111.0000 -150.0000 106

 11 omega   19.00   93.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.9365   57.0000  120.0000 148

 12 omega   66.00   94.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -45.0000  -90.0000 56

 13 omega   21.00   62.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -94.0000   60.0000 82

 14 omega   68.00   94.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -94.0000   60.0000 52

 15 omega   27.00   71.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -30.0000   60.0000 88

 16 omega   92.00  156.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -15.0000  -60.0000 128

 17 omega   38.00   75.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1716  -15.0000  -60.0000 74
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0154685000
_diffrn_orient_matrix_UB_12      0.0800536000
_diffrn_orient_matrix_UB_13      -0.0161520000
_diffrn_orient_matrix_UB_21      0.0833404000
_diffrn_orient_matrix_UB_22      -0.0204042000
_diffrn_orient_matrix_UB_23      -0.0089430000
_diffrn_orient_matrix_UB_31      -0.0204505000
_diffrn_orient_matrix_UB_32      -0.0227133000
_diffrn_orient_matrix_UB_33      -0.0488999000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            39981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.642
_diffrn_reflns_theta_min         3.507
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.595
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.296
_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)
followed ba ABSPACK
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.1942
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.0589
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
 
 Hooft parameter: -0.005(4)
Parsons quotient method : -0.003(1)

;
_refine_ls_abs_structure_Flack   -0.005(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1260
_refine_ls_number_reflns         18189
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+5.4721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                16578
_reflns_number_total             18189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             7031639
_cod_data_source_file            c4dt01590h2.cif
_cod_data_source_block           9
_cod_original_cell_volume        9363.21(15)
_cod_database_code               7031893
_chemical_oxdiff_formula         ' Mn4 Cl10 O20 C86 N18 H76'
_reflns_odcompleteness_completeness 99.90
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N11C-H11C = N11B-H11B = N11D-H11D = N11A-H11A
 0.87 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C2D(H2D), C2B(H2B), C2A(H2A), C2C(H2C)
3.b Secondary CH2 refined with riding coordinates:
 C12C(H12A,H12B), C12B(H12C,H12D), C12D(H12E,H12F), C12A(H12G,H12H), C3(H3B,
 H3A), C2(H2E,H2F), C4(H4A,H4B), C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C16C(H16C), C5F(H5F), C16A(H16A), C19C(H19C), C9F(H9F), C7D(H7D), C16B(H16B),
 C18A(H18A), C6C(H6C), C17D(H17D), C8D(H8D), C6F(H6F), C17B(H17B), C8B(H8B),
 C18C(H18C), C7C(H7C), C17C(H17C), C6D(H6D), C6A(H6A), C7F(H7F), C5E(H5E),
 C16D(H16D), C19A(H19A), C7A(H7A), C17A(H17A), C6B(H6B), C9E(H9E), C7E(H7E),
 C9B(H9B), C8C(H8C), C9C(H9C), C6E(H6E), C7B(H7B), C18D(H18D), C9D(H9D),
 C19D(H19D), C18B(H18B), C8A(H8A), C9A(H9A), C19B(H19B)
3.d Idealised Me refined as rotating group:
 C22D(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C22A(H22G,H22H,H22I), C22C(H22J,
 H22K,H22L)
;
_shelxl_version_number           2013-4