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_4127516
_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, Cl O3, 2.42(O)'
_chemical_formula_sum            'C50 H51.85 Cl Co4 N8 O20.42'
_chemical_formula_weight         1362.81
_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             2019-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.0964(15)
_cell_angle_beta                 105.6172(15)
_cell_angle_gamma                92.2521(14)
_cell_formula_units_Z            2
_cell_length_a                   12.7097(2)
_cell_length_b                   14.2447(3)
_cell_length_c                   15.7479(3)
_cell_measurement_reflns_used    30773
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      28.2560
_cell_measurement_theta_min      2.3890
_cell_volume                     2743.49(9)
_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_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 0.998
_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    -29.00  63.00   0.50   60.00    --   -6.30  77.00 -90.00  184
  2  \w    -19.00  71.00   0.50   60.00    --   -6.30  38.00-150.00  180
  3  \w    -27.00  39.00   0.50   60.00    --    5.36 -99.00  30.00  132
  4  \w    -27.00  27.00   0.50   60.00    --   -6.30 -99.00   0.00  108
  5  \w    -27.00  27.00   0.50   60.00    --   -6.30 -99.00  90.00  108
  6  \w    -72.00  18.00   0.50   60.00    --    5.36 -38.00  90.00  180
  7  \w    -27.00  27.00   0.50   60.00    --   -6.30 -99.00-180.00  108
  8  \w    -85.00   7.00   0.50   60.00    --   -6.30 -19.00-120.00  184
  9  \w    -74.00  85.00   0.50   60.00    --    5.36   0.00 120.00  318
;
_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      0.0513369000
_diffrn_orient_matrix_UB_12      -0.0020843000
_diffrn_orient_matrix_UB_13      0.0318072000
_diffrn_orient_matrix_UB_21      -0.0026133000
_diffrn_orient_matrix_UB_22      0.0480387000
_diffrn_orient_matrix_UB_23      0.0108671000
_diffrn_orient_matrix_UB_31      -0.0268576000
_diffrn_orient_matrix_UB_32      -0.0130998000
_diffrn_orient_matrix_UB_33      0.0325232000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69741
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.656
_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    1.650
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13568
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0663P)^2^+2.5517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11415
_reflns_number_total             13568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891287(1-3oac-clo3final)
_cod_original_cell_volume        2743.48(8)
_cod_database_code               4127516
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H53 Cl Co4 N8 O21'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 O19B-O18B
 2.37 with sigma of 0.005
 O18B-O20B
 2.37 with sigma of 0.005
 O20B-O19B
 2.37 with sigma of 0.005
 O11B-C45B \\sim O11A-C45A
 with sigma of 0.005
 Co2-O10B \\sim Co2-O10A
 with sigma of 0.005
 O10B-C45B \\sim O10A-C45A
 with sigma of 0.005
 C46B-C45B \\sim C46A-C45A
 with sigma of 0.005
 Cl1B-O18B \\sim Cl1B-O20B \\sim Cl1B-O19B \\sim Cl1A-O18A \\sim Cl1A-O19A
\\sim Cl1A-O20A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O10A \\sim O10B \\sim O11A \\sim O11B \\sim C45A \\sim C45B \\sim C46A \\sim
C46B: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
O18B \\sim O20A \\sim O19A \\sim O18A \\sim Cl1A \\sim Cl1B \\sim O19B \\sim
O20B: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 O10A, O10B, O11A, O11B, C45A, C45B, C46A, C46B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 Cl1A, Cl1B, O17, O18A, O18B, O19A, O19B, O20A, O20B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1B)=Sof(O18B)=Sof(O19B)=Sof(O20B)=1-FVAR(1)
 Sof(Cl1A)=Sof(O17)=Sof(O18A)=Sof(O19A)=Sof(O20A)=FVAR(1)
 Sof(O10B)=Sof(O11B)=Sof(C45B)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(2)
 Sof(O10A)=Sof(O11A)=Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(2)
 Fixed Sof: O21(0.6)
6.a 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)
6.b Idealised Me refined as rotating group:
 C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C)
6.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8)
;
_shelx_hkl_checksum              68422
_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 1.960
_oxdiff_exptl_absorpt_empirical_full_min 0.635