Mechanistically Driven Control over Cubane Oxo Cluster Catalysts.
Song, Fangyuan; Al-Ameed, Karrar; Schilling, Mauro; Fox, Thomas; Luber, Sandra; Patzke, Greta R.; Journal of the American Chemical Society 141 (2019) 8846–8857; doi:10.1021/jacs.9b01356

data_4127523
_publ_section_title
;
 Mechanistically Driven Control over Cubane Oxo Cluster Catalysts.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8846
_journal_page_last               8857
_journal_paper_doi               10.1021/jacs.9b01356
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'C66 H53 Co5 N12 O12, 3.61(H2 O), 3(N O3), 4.89(O)'
_chemical_formula_sum            'C66 H60.21 Co5 N15 O29.5'
_chemical_formula_weight         1830.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.2810(10)
_cell_angle_beta                 92.0850(10)
_cell_angle_gamma                107.5810(10)
_cell_formula_units_Z            2
_cell_length_a                   11.93210(10)
_cell_length_b                   13.38640(10)
_cell_length_c                   23.8027(2)
_cell_measurement_reflns_used    25567
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      78.2310
_cell_measurement_theta_min      3.4660
_cell_volume                     3619.75(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -74.00  19.00   0.50    1.50    --  -51.91  77.00  30.00  186
  2  \w    -62.00 -24.00   0.50    6.00    --  -84.25  30.00-150.00   76
  3  \w   -119.00 -45.00   0.50    1.50    --  -51.91 -57.00-150.00  148
  4  \w   -125.00 -54.00   0.50    1.50    --  -51.91 -38.00 -30.00  142
  5  \w    -84.00 -15.00   0.50    6.00    --  -84.25 111.00  30.00  138
  6  \w   -122.00 -38.00   0.50    1.50    --  -51.91 -57.00 -90.00  168
  7  \w   -126.00 -73.00   0.50    1.50    --  -51.91-125.00-180.00  106
  8  \w   -112.00 -82.00   0.50    1.50    --  -51.91-125.00 120.00   60
  9  \w     36.00  63.00   0.50    6.00    --  105.75-111.00  90.00   54
 10  \w     82.00 112.00   0.50    6.00    --  105.75-111.00  60.00   60
 11  \w     83.00 109.00   0.50    6.00    --  105.75 -94.00   0.00   52
 12  \w     88.00 118.00   0.50    6.00    --  105.75 -61.00 -60.00   60
 13  \w     77.00 103.00   0.50    6.00    --  105.75 -94.00-120.00   52
 14  \w     97.00 127.00   0.50    6.00    --  105.75 -77.00-150.00   60
 15  \w     71.00 110.00   0.50    6.00    --  105.75-111.00 -60.00   78
 16  \w     86.00 112.00   0.50    6.00    --  105.75-111.00 -30.00   52
 17  \w     86.00 112.00   0.50    6.00    --  105.75-111.00  30.00   52
 18  \w     74.00 116.00   0.50    6.00    --  105.75 -61.00  60.00   84
 19  \w     73.00 109.00   0.50    6.00    --  105.75-111.00   0.00   72
 20  \w     77.00 125.00   0.50    6.00    --  105.75 -77.00  30.00   96
 21  \w     75.00 112.00   0.50    6.00    --  105.75-111.00  90.00   74
 22  \w     87.00 113.00   0.50    6.00    --  105.75 -77.00 150.00   52
 23  \w     71.00 110.00   0.50    6.00    --  105.75-111.00 150.00   78
 24  \w     78.00 104.00   0.50    6.00    --  105.75 -94.00  90.00   52
 25  \w     60.00  94.00   0.50    6.00    --  105.75 -94.00 150.00   68
 26  \w     43.00  75.00   0.50    6.00    --  105.75 -45.00  60.00   64
 27  \w     35.00  69.00   0.50    6.00    --  105.75 -61.00  60.00   68
 28  \w     39.00  74.00   0.50    6.00    --  105.75 -61.00  30.00   70
 29  \w     32.00  77.00   0.50    6.00    --  105.75 -45.00 -30.00   90
 30  \w     78.00 119.00   0.50    6.00    --  105.75 -61.00 -90.00   82
 31  \w     79.00 109.00   0.50    6.00    --  105.75 -94.00-150.00   60
 32  \w     74.00 125.00   0.50    6.00    --  105.75-136.00-106.58  102
 33  \w     44.00  94.00   0.50    6.00    --  105.75 -94.00 -60.00  100
 34  \w     47.00  72.00   0.50    6.00    --  105.75 -94.00-120.00   50
 35  \w     43.00  84.00   0.50    6.00    --  105.75 -94.00-180.00   82
 36  \w     28.00  63.00   0.50    6.00    --  105.75 -30.00-120.00   70
 37  \w     35.00  62.00   0.50    6.00    --  105.75 -30.00 -90.00   54
 38  \w     32.00  69.00   0.50    6.00    --  105.75 -30.00 -30.00   74
 39  \w     96.00 123.00   0.50    6.00    --  105.75  15.00   0.00   54
 40  \w    133.00 176.00   0.50    6.00    --  105.75  15.00   0.00   86
 41  \w    106.00 140.00   0.50    6.00    --  105.75  30.00  60.00   68
 42  \w    109.00 135.00   0.50    6.00    --  105.75  15.00  60.00   52
 43  \w     91.00 168.00   0.50    6.00    --  105.75  61.00  60.00  154
 44  \w    146.00 172.00   0.50    6.00    --  105.75 111.00   0.00   52
 45  \w    144.00 175.00   0.50    6.00    --  105.75 111.00 -60.00   62
 46  \w    109.00 134.00   0.50    6.00    --  105.75  15.00-120.00   50
 47  \w    147.00 173.00   0.50    6.00    --  105.75  15.00-120.00   52
 48  \w     99.00 132.00   0.50    6.00    --  105.75 111.00   0.00   66
 49  \w    100.00 142.00   0.50    6.00    --  105.75 111.00  60.00   84
 50  \w    143.00 178.00   0.50    6.00    --  105.75 111.00  90.00   70
 51  \w    109.00 178.00   0.50    6.00    --  105.75  45.00 150.00  138
 52  \w    102.00 147.00   0.50    6.00    --  105.75  15.00 150.00   90
 53  \w     99.00 132.00   0.50    6.00    --  105.75 111.00 -60.00   66
 54  \w    100.00 151.00   0.50    6.00    --  105.75 178.00 -90.00  102
 55  \w     97.00 103.50   0.50    6.00    --  105.75 178.00 120.00   13
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1107675000
_diffrn_orient_matrix_UB_12      0.0204859000
_diffrn_orient_matrix_UB_13      0.0225206000
_diffrn_orient_matrix_UB_21      -0.0153883000
_diffrn_orient_matrix_UB_22      -0.0916488000
_diffrn_orient_matrix_UB_23      0.0399810000
_diffrn_orient_matrix_UB_31      0.0766460000
_diffrn_orient_matrix_UB_32      0.0759781000
_diffrn_orient_matrix_UB_33      0.0457604000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            60044
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.379
_diffrn_reflns_theta_min         3.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.644
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1204
_refine_ls_number_reflns         15055
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0585P)^2^+2.7370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12855
_reflns_number_total             15055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891334(2-Co5-NO3final)
_cod_original_formula_sum        'C66 H60.21 Co5 N15 O29.50'
_cod_database_code               4127523
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C66 H59 Co5 N14 O26'
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O32-N17 = O31A-N17 = O30A-N17
 1.27 with sigma of 0.005
 O26A-N16B = O25A-N16B = O24A-N16B
 1.27 with sigma of 0.005
 O26B-O25B
 2.17 with sigma of 0.005
 O18-O19
 2.17 with sigma of 0.005
 O19-O17
 2.17 with sigma of 0.005
 O17-O18
 2.17 with sigma of 0.005
 O24A-O26A
 2.17 with sigma of 0.005
 O31A-O32
 2.17 with sigma of 0.005
 O30A-O31A
 2.17 with sigma of 0.005
 O32-O30A
 2.17 with sigma of 0.005
 O26B-O24B
 2.17 with sigma of 0.005
 O24B-O25B
 2.17 with sigma of 0.005
 O25A-O24A
 2.17 with sigma of 0.005
 O25A-O26A
 2.17 with sigma of 0.005
 O18-N14 \\sim O19-N14 \\sim O17-N14
 with sigma of 0.005
 O26B-N16A \\sim O24B-N16A \\sim O25B-N16A
 with sigma of 0.005
3. Restrained planarity
 O24A, O25A, O26A, N16B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
O14 \\sim O15 \\sim O16: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
O17 \\sim O18 \\sim O19: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
O24B \\sim O25B \\sim O26B: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
O24A \\sim O25A \\sim O26A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 O14, O15, O16, N13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O17, O18, O19, N14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O24B, O25B, O26B, N16A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O24A, O25A, O26A, N16B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O20B)=1-FVAR(1)
 Sof(O20A)=FVAR(1)
 Sof(O29B)=1-FVAR(2)
 Sof(O29A)=Sof(H29A)=Sof(H29B)=FVAR(2)
 Sof(O33B)=1-FVAR(3)
 Sof(O33A)=FVAR(3)
 Fixed Sof: O14(0.5) O14B(0.5) H14A(0.5) H14B(0.5) O15(0.5) O16(0.5) O17(0.3)
 O18(0.3) O18B(0.5) O19(0.3) O24A(0.4) O24B(0.4) O25A(0.4) O25B(0.4) O26A(0.4)
 O26B(0.4) O27A(0.5) O27B(0.5) O28(0.4) O30A(0.4) O30B(0.3) O31A(0.4) O31B(0.3)
 O32(0.4) O038(0.5) H03A(0.5) H03B(0.5) N13(0.5) N14(0.3) N16A(0.4) N16B(0.4)
 N17(0.4)
7.a Free rotating group:
 O010(H01A,H01B), O13(H13A,H13B), O14B(H14A,H14B), O29A(H29A,H29B), O038(H03A,
 H03B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8A), C9(H9), C10(H10), C11(H11A),
 C12(H12A), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C63(H63),
 C64(H64), C65(H65), C66(H66)
7.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O7(H7), O8(H8), O11(H11), O12(H12)
;
_shelx_hkl_checksum              53302
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.785