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_4127524
_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, 2(H2 O), 19(O)'
_chemical_formula_sum            'C52 H90 Co4 N8 O37'
_chemical_formula_weight         1655.03
_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             2019-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                63.079(2)
_cell_angle_beta                 70.4300(10)
_cell_angle_gamma                65.817(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7712(2)
_cell_length_b                   17.5108(3)
_cell_length_c                   17.9137(2)
_cell_measurement_reflns_used    54389
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      30.4600
_cell_measurement_theta_min      2.3710
_cell_volume                     3704.60(12)
_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      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_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    -27.00  52.00   0.50   10.00    --   20.22 -99.00  90.00  158
  2  \w     35.00  99.00   0.50   10.00    --   20.22-178.00  90.00  128
  3  \w     35.00  99.00   0.50   10.00    --   20.22-178.00-120.00  128
  4  \w    -27.00  52.00   0.50   10.00    --   20.22 -99.00 -60.00  158
  5  \w    -27.00  52.00   0.50   10.00    --   20.22 -99.00-120.00  158
  6  \w    -31.00  55.00   0.50   10.00    --  -21.78  38.00  30.00  172
  7  \w     38.00  98.00   0.50   10.00    --   20.22 178.00-180.00  120
  8  \w     38.00  98.00   0.50   10.00    --   20.22 178.00  30.00  120
  9  \w    -94.00  -8.00   0.50   10.00    --  -21.78 -57.00 -30.00  172
 10  \w    -94.00  -8.00   0.50   10.00    --  -21.78 -57.00 120.00  172
 11  \w    -27.00  -2.00   0.50   10.00    --   20.22 -99.00 150.00   50
 12  \w    -95.00   0.00   0.50   10.00    --  -21.78 -77.00 120.00  190
 13  \w    -95.00   0.00   0.50   10.00    --  -21.78 -77.00 -90.00  190
 14  \w    -94.00  -8.00   0.50   10.00    --  -21.78 -57.00-150.00  172
 15  \w    -99.00 -13.00   0.50   10.00    --  -21.78 -38.00-120.00  172
 16  \w    -99.00 -13.00   0.50   10.00    --  -21.78 -38.00   0.00  172
;
_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      0.0423496000
_diffrn_orient_matrix_UB_12      -0.0304425000
_diffrn_orient_matrix_UB_13      0.0195914000
_diffrn_orient_matrix_UB_21      0.0105025000
_diffrn_orient_matrix_UB_22      0.0365653000
_diffrn_orient_matrix_UB_23      -0.0010332000
_diffrn_orient_matrix_UB_31      -0.0310467000
_diffrn_orient_matrix_UB_32      -0.0038700000
_diffrn_orient_matrix_UB_33      0.0406949000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            139318
_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         30.508
_diffrn_reflns_theta_min         2.186
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.484
_exptl_crystal_description       plate
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.016
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         22603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0594
_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^)+(0.1048P)^2^+5.1120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17218
_reflns_number_total             22603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891335(1-4OAc(evolved))
_cod_database_code               4127524
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C86 H106 Co8 N50 O38 '
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.829
_reflns_odcompleteness_completeness 62.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_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. Others
 Sof(O25B)=1-FVAR(1)
 Sof(O25A)=FVAR(1)
 Sof(O37A)=1-FVAR(2)
 Sof(O37B)=FVAR(2)
 Sof(O21A)=1-FVAR(3)
 Sof(O21B)=FVAR(3)
 Sof(O38B)=1-FVAR(4)
 Sof(O38A)=FVAR(4)
 Sof(O33B)=1-FVAR(5)
 Sof(O33A)=FVAR(5)
 Fixed Sof: O28(0.5) O29(0.5)
3.a Free rotating group:
 O17(H17A,H17B), O20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8A), C9(H9), C10(H10), C11(H11), C12(H12),
  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)
3.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8)
;
_shelx_hkl_checksum              74767
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.766