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_4127519
_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         'C48 H46 Co4 N8 O14, 2(N1 O3)'
_chemical_formula_sum            'C48 H46 Co4 N10 O20'
_chemical_formula_weight         1318.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.258(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5898(6)
_cell_length_b                   11.9550(2)
_cell_length_c                   21.4009(6)
_cell_measurement_reflns_used    12904
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      77.9620
_cell_measurement_theta_min      4.2880
_cell_volume                     5183.2(3)
_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      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -61.00  25.00   0.50    6.50    --  -51.91  38.00   0.00  172
  2  \w    -25.00  61.00   0.50    6.50    --   51.91 -38.00  60.00  172
  3  \w     30.00  77.00   0.50   26.00    --  105.75 -45.00 -30.00   94
  4  \w     35.00 121.00   0.50   26.00    --  105.75 -61.00  30.00  172
  5  \w     96.00 178.00   0.50   26.00    --  105.75  15.00  90.00  164
  6  \w     97.00 178.00   0.50   26.00    --  105.75  30.00 120.00  162
  7  \w     99.00 178.00   0.50   26.00    --  105.75 111.00 120.00  158
  8  \w     99.00 178.00   0.50   26.00    --  105.75 111.00-120.00  158
  9  \w     96.00 178.00   0.50   26.00    --  105.75  15.00-120.00  164
 10  \w     59.00 151.00   0.50   26.00    --  105.75 178.00 120.00  184
 11  \w     28.00  69.00   0.50   26.00    --  105.75 -30.00 -90.00   82
 12  \w     28.00  69.00   0.50   26.00    --  105.75 -30.00 -30.00   82
 13  \w     31.00 131.00   0.50   26.00    --  105.75 -85.00  -2.00  200
 14  \w     39.00  68.00   0.50   26.00    --  105.75 -45.00 150.00   58
 15  \w     28.00  69.00   0.50   26.00    --  105.75 -30.00  90.00   82
 16  \w     30.00  77.00   0.50   26.00    --  105.75 -45.00  60.00   94
 17  \w     30.00  99.00   0.50    6.50    --   51.91-125.00 -30.00  138
 18  \w     30.00  77.00   0.50   26.00    --  105.75 -45.00  30.00   94
 19  \w     28.00  69.00   0.50   26.00    --  105.75 -30.00-180.00   82
 20  \w     30.00  77.00   0.50   26.00    --  105.75 -45.00-180.00   94
 21  \w   -129.00 -43.00   0.50    6.50    --  -51.91 -38.00 -30.00  172
 22  \w   -126.00 -70.00   0.50    6.50    --  -51.91-125.00 -90.00  112
 23  \w   -127.00 -82.00   0.50    6.50    --  -51.91 -99.00  60.00   90
;
_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      0.0666367000
_diffrn_orient_matrix_UB_12      0.0620784000
_diffrn_orient_matrix_UB_13      0.0301967000
_diffrn_orient_matrix_UB_21      -0.0303778000
_diffrn_orient_matrix_UB_22      0.0955527000
_diffrn_orient_matrix_UB_23      0.0246463000
_diffrn_orient_matrix_UB_31      0.0204052000
_diffrn_orient_matrix_UB_32      -0.0602400000
_diffrn_orient_matrix_UB_33      0.0701487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27903
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.484
_diffrn_reflns_theta_min         4.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.631
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.589
_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            'metallic pinkish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       plate
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0507
_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^)+(0.1078P)^2^+6.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4649
_reflns_number_total             5291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891290(2-Co4-NO3final)
_cod_original_cell_volume        5183.2(2)
_cod_database_code               4127519
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H46 Co4 N10 O20'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9A-O10A
 2.15 with sigma of 0.005
 O9A-O8A
 2.15 with sigma of 0.005
 O8A-O10A
 2.15 with sigma of 0.005
 O9B-O10B
 2.15 with sigma of 0.005
 O9B-O8B
 2.15 with sigma of 0.005
 O10B-O8B
 2.15 with sigma of 0.005
 Co1-O6B \\sim Co1-O6A
 with sigma of 0.005
 O6B-C23A \\sim O6A-C23B
 with sigma of 0.005
 O7A-C23A \\sim O7B-C23B
 with sigma of 0.005
 C23A-C24A \\sim C24B-C23B
 with sigma of 0.005
 O9B-N5B \\sim O9A-N5A \\sim O8A-N5A \\sim O10A-N5A \\sim O10B-N5B \\sim O8B-N5B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O6A \\sim O6B \\sim O7A \\sim O7B \\sim C23A \\sim C23B \\sim C24A \\sim C24B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.08
O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B \\sim N5A \\sim N5B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O6A, O6B, O7A, O7B, C23A, C23B, C24A, C24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O8A, O8B, O9A, O9B, O10A, O10B, N5A, N5B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O6B)=Sof(O7B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(O6A)=Sof(O7A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(N5B)=1-FVAR(2)
 Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(N5A)=FVAR(2)
6.a Rotating group:
 O5(H5A)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22)
6.c Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_shelx_hkl_checksum              60696
_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 1.646
_oxdiff_exptl_absorpt_empirical_full_min 0.683