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_4127521
_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
'C52 H48 Co4 N8 O16, 3.41(C2 H6 O), 0.59(C2 H5 O)'
_chemical_formula_sum            'C60 H72 Co4 N8 O20'
_chemical_formula_weight         1460.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.059(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6067(10)
_cell_length_b                   14.0325(6)
_cell_length_c                   18.7571(12)
_cell_measurement_reflns_used    5789
_cell_measurement_temperature    184(3)
_cell_measurement_theta_max      25.3910
_cell_measurement_theta_min      2.6740
_cell_volume                     3188.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      184(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_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   -101.00 -75.00   1.00  100.00    --  -11.40-178.00  60.00   26
  2  \w    -99.00 -58.00   1.00  100.00    --  -11.40 178.00 120.00   41
  3  \w     51.00  77.00   1.00  100.00    --  -11.40-178.00   0.00   26
  4  \w     -9.00  16.00   1.00  100.00    --   12.18 104.00 155.00   25
  5  \w     -8.00  47.00   1.00  100.00    --   12.18  57.00   0.00   55
  6  \w    -34.00  86.00   1.00  100.00    --   12.18  19.00 120.00  120
  7  \w     -2.00  76.00   1.00  100.00    --   12.18   0.00  30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0487703000
_diffrn_orient_matrix_UB_12      0.0114441000
_diffrn_orient_matrix_UB_13      -0.0100833000
_diffrn_orient_matrix_UB_21      0.0321859000
_diffrn_orient_matrix_UB_22      -0.0114652000
_diffrn_orient_matrix_UB_23      0.0363725000
_diffrn_orient_matrix_UB_31      0.0038581000
_diffrn_orient_matrix_UB_32      -0.0478620000
_diffrn_orient_matrix_UB_33      -0.0111225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28602
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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)
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    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6049
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0522P)^2^+4.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4326
_reflns_number_total             6049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891332(DefectCocubane)
_cod_database_code               4127521
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H65 Co4 N8 O20'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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, All O(H) groups
2. Restrained distances
 O10B-C29B = O10A-C29A
 1.45 with sigma of 0.005
 C29A-C30A = C29B-C30B
 1.48 with sigma of 0.005
 O4-H4
 0.86 with sigma of 0.005
 O10B-C30B
 2.32 with sigma of 0.005
 C29A-C30A \\sim C29B-C30B
 with sigma of 0.005
 O10B-C29B \\sim O10A-C29A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O10B \\sim C29B \\sim C29A \\sim O10A \\sim C30B \\sim C30A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.08
O10B \\sim O10A \\sim C29A \\sim C29B \\sim C30B \\sim C30A: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O10B, O10A, C29A, C29B, C30B, C30A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 C30A, C30B, C29A, C29B, O10B, O10A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29B)=Sof(H29C)=Sof(H29D)=
 Sof(O10B)=1-FVAR(1)
 Sof(O10A)=Sof(H10A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C29A(H29A,H29B), C27(H27A,H27B), C29B(H29C,H29D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4A), C8(H8), C19(H19), C22(H22), C3(H3A), C11(H11), C20(H20), C21(H21),
 C9(H9), C10(H10), C1(H1), C15(H15), C12(H12), C2(H2), C14(H14), C13(H13)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C30A(H30A,H30B,H30C), C28(H28A,H28B,
 H28C), C30B(H30D,H30E,H30F)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O9(H9A), O10A(H10A)
;
_shelx_hkl_checksum              73773
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.806