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_4127514
_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, F6 P, H2 O, 0.41(C H4 O), C0.09 H0.26 O0.04'
_chemical_formula_sum            'C50.5 H51 Co4 F6 N8 O16.5 P'
_chemical_formula_weight         1414.68
_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                89.681(2)
_cell_angle_beta                 72.126(2)
_cell_angle_gamma                86.839(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9163(4)
_cell_length_b                   14.1420(3)
_cell_length_c                   16.2926(4)
_cell_measurement_reflns_used    34044
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      28.2380
_cell_measurement_theta_min      2.5950
_cell_volume                     2827.89(13)
_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 0.999
_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     -7.00  86.00   0.50   50.00    --    5.52  19.00 120.00  186
  2  \w     -7.00  83.00   0.50   50.00    --    5.52  38.00 -30.00  180
  3  \w     -7.00  83.00   0.50   50.00    --    5.52  38.00-150.00  180
  4  \w     38.00  85.00   0.50   50.00    --    5.52 178.00-120.00   94
  5  \w     38.00  85.00   0.50   50.00    --    5.52 178.00  60.00   94
  6  \w     38.00  85.00   0.50   50.00    --    5.52 178.00  90.00   94
  7  \w    -19.00  71.00   0.50   50.00    --   -6.45  38.00 -90.00  180
  8  \w    -27.00  39.00   0.50   50.00    --    5.52 -99.00-150.00  132
  9  \w    -27.00  27.00   0.50   50.00    --   -6.45 -99.00   0.00  108
 10  \w    -27.00  27.00   0.50   50.00    --   -6.45 -99.00  90.00  108
 11  \w    -27.00  -3.50   0.50   50.00    --    5.52 -99.00 150.00   47
;
_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      -0.0438865000
_diffrn_orient_matrix_UB_12      -0.0102931000
_diffrn_orient_matrix_UB_13      0.0369161000
_diffrn_orient_matrix_UB_21      -0.0357400000
_diffrn_orient_matrix_UB_22      0.0299465000
_diffrn_orient_matrix_UB_23      -0.0153482000
_diffrn_orient_matrix_UB_31      -0.0116811000
_diffrn_orient_matrix_UB_32      -0.0389984000
_diffrn_orient_matrix_UB_33      -0.0222338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64949
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.660
_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    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         14037
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0491P)^2^+3.1456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11924
_reflns_number_total             14037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891285(1-3oac-pf6final)
_cod_original_cell_volume        2827.90(13)
_cod_original_formula_sum        'C50.50 H51 Co4 F6 N8 O16.50 P'
_cod_database_code               4127514
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H49 Co4 F6 N8 O16 P'
_reflns_odcompleteness_completeness 99.88
_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
 F6A-F5A
 2.2 with sigma of 0.01
 F1A-F5A
 2.2 with sigma of 0.008
 F1A-F3A
 2.2 with sigma of 0.01
 F3A-F6A
 2.2 with sigma of 0.008
 F6A-F4A
 2.2 with sigma of 0.01
 F6A-F2A
 2.2 with sigma of 0.01
 F2A-F5A
 2.2 with sigma of 0.01
 F1A-F4A
 2.2 with sigma of 0.01
 F2A-F1A
 2.2 with sigma of 0.01
 F4A-F5A
 2.2 with sigma of 0.01
 F3B-F6B
 2.2 with sigma of 0.01
 F6B-F5B
 2.2 with sigma of 0.01
 F1B-F5B
 2.2 with sigma of 0.01
 F3B-F1B
 2.2 with sigma of 0.01
 F6B-F2B
 2.2 with sigma of 0.01
 F4B-F6B
 2.2 with sigma of 0.01
 F1B-F4B
 2.2 with sigma of 0.01
 F1B-F2B
 2.2 with sigma of 0.01
 P1-F4A \\sim P1-F4B \\sim P1-F1B \\sim P1-F5B \\sim P1-F5A \\sim P1-F2B \\sim
P1-F2A \\sim P1-F6B \\sim P1-
 F3B \\sim P1-F3A \\sim P1-F6A \\sim P1-F1A
 with sigma of 0.002
 O17-C51 \\sim O18-C52
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O18 \\sim C52 \\sim C51 \\sim O17: within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.005
F3A \\sim F3B \\sim F2B \\sim F2A \\sim F6B \\sim F6A \\sim F5A \\sim F5B \\sim
F1A \\sim F1B \\sim F4B \\sim F4A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 P1, F1A, F1B, F2A, F2B, F3A, F3B, F4A, F4B, F5A, F5B, F6A, F6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Sof(C52)=Sof(H52a)=Sof(H52b)=Sof(H52c)=0.5*(1-FVAR(3))
 Sof(O18)=0.25*(1-FVAR(3))
 Sof(O17)=Sof(H17)=Sof(C51)=Sof(H51a)=Sof(H51b)=Sof(H51c)=0.5*FVAR(3)
6.a Free rotating group:
 O16(H16a,H16b)
6.b Rotating group:
 O9(H9a,H9b)
6.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)
6.d Idealised Me refined as rotating group:
 C46(H46a,H46b,H46c), C48(H48a,H48b,H48c), C50(H50a,H50b,H50c), C51(H51a,H51b,
 H51c), C52(H52a,H52b,H52c)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8), O17(H17)
;
_shelx_hkl_checksum              11925
_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 1.569
_oxdiff_exptl_absorpt_empirical_full_min 0.581