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_4127517
_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         'C48 H46 Co4 N8 O14, 2(B F4)'
_chemical_formula_sum            'C48 H46 B2 Co4 F8 N8 O14'
_chemical_formula_weight         1368.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.784(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6584(5)
_cell_length_b                   12.1359(3)
_cell_length_c                   21.1615(5)
_cell_measurement_reflns_used    25123
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      27.9800
_cell_measurement_theta_min      2.5280
_cell_volume                     5239.7(3)
_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      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      2.00  92.00   0.50   18.47    --   15.05  38.00  30.00  180
  2  \w      0.00  88.00   0.50   18.47    --   15.05  57.00 120.00  176
  3  \w     38.00  94.00   0.50   18.47    --   15.05 178.00-120.00  112
  4  \w     38.00  94.00   0.50   18.47    --   15.05 178.00-180.00  112
  5  \w    -58.00 -14.00   0.50   18.47    --   15.05 -57.00   0.00   88
  6  \w    -59.00  38.00   0.50   18.47    --   15.05 -77.00 -90.00  194
  7  \w    -27.00  48.00   0.50   18.47    --   15.05 -99.00-150.00  150
  8  \w     35.00  94.00   0.50   18.47    --   15.05-178.00-150.00  118
;
_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      -0.0002603000
_diffrn_orient_matrix_UB_12      0.0173075000
_diffrn_orient_matrix_UB_13      -0.0321409000
_diffrn_orient_matrix_UB_21      -0.0264803000
_diffrn_orient_matrix_UB_22      -0.0362399000
_diffrn_orient_matrix_UB_23      -0.0185800000
_diffrn_orient_matrix_UB_31      -0.0225137000
_diffrn_orient_matrix_UB_32      0.0424773000
_diffrn_orient_matrix_UB_33      -0.0027894000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39800
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.735
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.619
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+17.5062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5418
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891288(2-Co4-BF4final)
_cod_original_cell_volume        5239.7(2)
_cod_database_code               4127517
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H74 B2 Co4 F8 N12 O6'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 O7-H7B
 0.85 with sigma of 0.02
 O7-H7A
 0.85 with sigma of 0.02
 O3-H3
 0.85 with sigma of 0.001
 F3B-F4B
 2.26 with sigma of 0.005
 F4B-F2B
 2.26 with sigma of 0.005
 F3B-F2B
 2.26 with sigma of 0.005
 F1A-F3A
 2.26 with sigma of 0.005
 F1A-F4A
 2.26 with sigma of 0.005
 F1A-F2A
 2.26 with sigma of 0.005
 F3A-F2A
 2.26 with sigma of 0.005
 F2A-F4A
 2.26 with sigma of 0.005
 F4A-F3A
 2.26 with sigma of 0.005
 O6B-C24B
 2.37 with sigma of 0.005
 O6A-C24A
 2.37 with sigma of 0.005
 O5B-C24B
 2.37 with sigma of 0.005
 C24A-O5A
 2.37 with sigma of 0.005
 F1B-F2B
 2.26 with sigma of 0.005
 F4B-F1B
 2.26 with sigma of 0.005
 F3B-F1B
 2.26 with sigma of 0.005
 O6A-C23A \\sim O6B-C23B
 with sigma of 0.005
 C24A-C23A \\sim C23B-C24B
 with sigma of 0.005
 Co1-O5A \\sim Co1-O5B
 with sigma of 0.005
 O5A-C23A \\sim O5B-C23B
 with sigma of 0.005
 F1A-B1A \\sim F3A-B1A \\sim F3B-B1B \\sim F2A-B1A \\sim F2B-B1B \\sim F1B-B1B
\\sim F4A-B1A \\sim F4B-B1B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O5A \\sim O5B \\sim O6A \\sim O6B \\sim C23A \\sim C23B \\sim C24A \\sim C24B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.08
F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim F4A \\sim F4B \\sim
B1A \\sim B1B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.08
4. Rigid body (RIGU) restrains
 O5A, O5B, O6A, O6B, C23A, C23B, C24A, C24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 F1A, F1B, F2A, F2B, F3A, F3B, F4A, F4B, B1A, B1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(B1B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=FVAR(1)
 Sof(O5B)=Sof(O6B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(O5A)=Sof(O6A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22)
6.b Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
6.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_hkl_checksum              62966
_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 1.140
_oxdiff_exptl_absorpt_empirical_full_min 0.929