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_4127513
_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         'C50 H47 Co4 N8 O15, B F4, H2 O'
_chemical_formula_sum            'C50 H51 B Co4 F4 N8 O17'
_chemical_formula_weight         1358.51
_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
_audit_creation_date             2018-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                89.780(3)
_cell_angle_beta                 73.273(4)
_cell_angle_gamma                86.642(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7299(4)
_cell_length_b                   14.2087(5)
_cell_length_c                   15.7489(8)
_cell_measurement_reflns_used    13035
_cell_measurement_temperature    183.05(10)
_cell_measurement_theta_max      26.2910
_cell_measurement_theta_min      2.6830
_cell_volume                     2723.1(2)
_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)'
_diffrn_ambient_temperature      183.05(10)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -10.00  74.00   1.00   50.00    --   20.59  60.00 106.54   84
  2  \w     -8.00  21.00   1.00   50.00    --   20.59  60.00 -12.39   29
  3  \w     70.00  95.00   1.00   50.00    --   20.59  60.00 -12.39   25
  4  \w     15.00  42.00   1.00   50.00    --   20.59  60.00 153.89   27
  5  \w      9.00  52.00   1.00   50.00    --   20.59  60.00 -80.52   43
  6  \w     10.00  35.00   1.00   50.00    --   20.59  60.00   4.65   25
  7  \w    -48.00 -12.00   1.00   50.00    --   20.59 -57.00  60.00   36
  8  \w    -53.00  50.00   1.00   50.00    --   20.59 -57.00 -60.00  103
  9  \w     -2.00  93.00   1.00   50.00    --   20.59  60.00-155.02   95
 10  \w    -53.00  50.00   1.00   50.00    --   20.59 -57.00  60.00  103
 11  \w    -53.00  50.00   1.00   50.00    --   20.59 -57.00-150.00  103
 12  \w     -6.00  96.00   1.00   50.00    --   20.59  38.00   0.00  102
 13  \w    -54.00 -19.00   1.00   50.00    --   20.59 -60.00  -4.16   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.701
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.721
_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 intense purple'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.144
_platon_squeeze_details
;) TITL 1-3oac-bf4P -1 R = 0.05 CELL 12.7299 14.2087 15.7489 89.78 73.27 86.64 SPGR P-1 C101 0.845 0.099 0.203 ! 1.55 eA-3 Q102 0.387 0.629 0.219 ! 1.26 eA-3 C103 0.907 0.008 0.040 ! 1.21 eA-3 Q104 0.409 0.800 0.344 ! 1.20 eA-3 Q105 0.236 0.621 0.437 ! 1.11 eA-3 C106 0.908 0.140 0.130 ! 1.03 eA-3 C107 0.869 0.061 0.129 ! 0.98 eA-3 Q108 0.168 0.759 0.315 ! 0.93 eA-3 Q109 0.218 0.844 0.221 ! 0.91 eA-3 Q110 0.419 0.723 0.120 ! 0.82 eA-3 Q111 0.924 0.261 0.301 ! 0.78 eA-3 C112 0.783 0.066 0.170 ! 0.75 eA-3 Q113 0.857 0.496 0.290 ! 0.73 eA-3 Q114 0.281 0.719 0.341 ! 0.72 eA-3 C115 0.952 0.985 0.095 ! 0.63 eA-3 Q116 0.921 0.277 0.207 ! 0.62 eA-3 Q117 0.893 0.200 0.165 ! 0.57 eA-3 Q118 0.795 0.607 0.479 ! 0.57 eA-3 Q119 0.203 0.552 0.226 ! 0.53 eA-3 Q120 0.015 0.811 0.355 ! 0.53 eA-3 C121 0.916 0.092 0.070 ! 0.53 eA-3 Q122 0.435 0.893 0.250 ! 0.52 eA-3 Q123 0.822 0.354 0.207 ! 0.51 eA-3 ) 
_shelx_fab_checksum                20262
_platon_squeeze_details            ?
_platon_squeeze_void_probe_radius  1.20
_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 
_vrf_CHEMW03_1-3oac-bf4_sq PROBLEM: The ratio of given/expected molecular weight as RESPONSE: 10 e/cavity per asymmetric unit was observed by using SQUEEZE, which equates 1 isolated water. The final refinement was based on such SQUEEZE result. However, such ignored water is still counted into UNIT, and the difference between given/expected molecular weight is caused by such scenario.
;
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         11133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0431P)^2^+4.8371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8885
_reflns_number_total             11133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891284(1-3oac-bf4_sq)
_cod_original_cell_volume        2723.13(19)
_cod_database_code               4127513
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.607
_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.a Free rotating group:
 O16(H16A,H16B)
2.b Rotating group:
 O9(H9A,H9B)
2.c 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)
2.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8)
;
_platon_squeeze_void_probe_radius 1.20