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_4127518
_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(Cl O3)'
_chemical_formula_sum            'C48 H46 Cl2 Co4 N8 O20'
_chemical_formula_weight         1361.55
_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             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.686(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3692(6)
_cell_length_b                   12.07776(19)
_cell_length_c                   21.0774(5)
_cell_measurement_reflns_used    6906
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      77.4360
_cell_measurement_theta_min      3.9590
_cell_volume                     5131.8(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.980
_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    -66.00  21.00   0.50    2.00    --  -51.66  57.00 -30.00  174
  2  \w     38.00 118.00   0.50    2.00    --   51.66  77.00 150.00  160
  3  \w    132.00 173.00   0.50    8.00    --  105.75  15.00 120.00   82
  4  \w     97.00 170.00   0.50    8.00    --  105.75  30.00   0.00  146
  5  \w    130.00 177.00   0.50    8.00    --  105.75  15.00 -30.00   94
  6  \w    142.00 177.00   0.50    8.00    --  105.75  61.00-120.00   70
  7  \w     97.00 133.00   0.50    8.00    --  105.75  30.00-180.00   72
  8  \w     91.00 136.00   0.50    8.00    --  105.75  61.00-120.00   90
  9  \w     97.00 129.00   0.50    8.00    --  105.75  61.00-180.00   64
 10  \w     77.00 116.00   0.50    8.00    --  105.75 -15.00 -30.00   78
 11  \w     72.00 109.00   0.50    8.00    --  105.75 -61.00  30.00   74
 12  \w     85.00 120.00   0.50    8.00    --  105.75 -77.00 120.00   70
 13  \w     95.00 121.00   0.50    8.00    --  105.75 -61.00 120.00   52
 14  \w     38.00  63.00   0.50    8.00    --  105.75 -15.00 -30.00   50
 15  \w     45.00  70.00   0.50    8.00    --  105.75 -45.00 -60.00   50
 16  \w     48.00  74.00   0.50    8.00    --  105.75 -45.00 -90.00   52
 17  \w     31.00  66.00   0.50    8.00    --  105.75 -45.00 -30.00   70
 18  \w     42.00  68.00   0.50    8.00    --  105.75 -61.00  30.00   52
 19  \w     33.00  68.00   0.50    8.00    --  105.75 -30.00   0.00   70
 20  \w     28.00  66.00   0.50    8.00    --  105.75 -30.00 -30.00   76
 21  \w     29.00  56.00   0.50    8.00    --  105.75 -30.00 -90.00   54
 22  \w     28.00  69.00   0.50    8.00    --  105.75 -30.00-180.00   82
 23  \w     32.00  94.00   0.50    8.00    --  105.75-111.00 -60.00  124
 24  \w     38.00  91.00   0.50    8.00    --  105.75 -61.00 120.00  106
 25  \w     50.00  77.00   0.50    8.00    --  105.75 -45.00 150.00   54
 26  \w     46.00  73.00   0.50    8.00    --  105.75 -45.00 120.00   54
 27  \w     35.00  61.00   0.50    8.00    --  105.75 -77.00 120.00   52
 28  \w     28.00  69.00   0.50    8.00    --  105.75 -30.00 150.00   82
 29  \w   -116.00 -90.00   0.50    2.00    --  -51.66 -99.00 120.00   52
 30  \w   -127.00 -82.00   0.50    2.00    --  -51.66 -99.00   0.00   90
 31  \w   -127.00-122.00   0.50    2.00    --  -51.66 -99.00 -30.00   10
;
_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      0.0134698000
_diffrn_orient_matrix_UB_12      0.0923654000
_diffrn_orient_matrix_UB_13      -0.0425519000
_diffrn_orient_matrix_UB_21      -0.0654997000
_diffrn_orient_matrix_UB_22      -0.0280753000
_diffrn_orient_matrix_UB_23      -0.0641448000
_diffrn_orient_matrix_UB_31      -0.0369597000
_diffrn_orient_matrix_UB_32      0.0833790000
_diffrn_orient_matrix_UB_33      0.0255511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21680
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.306
_diffrn_reflns_theta_min         4.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46861
_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    1.762
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1015P)^2^+8.7939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4458
_reflns_number_total             5405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891289(2-Co4-ClO3final)
_cod_original_cell_volume        5131.7(2)
_cod_database_code               4127518
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C192 H176 Cl8 Co16 N32 O80 '
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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
 0.9 with sigma of 0.02
 O8B-O9B
 2.37 with sigma of 0.005
 O9A-O10A
 2.37 with sigma of 0.005
 O8A-O9A
 2.37 with sigma of 0.005
 O10A-O8A
 2.37 with sigma of 0.005
 O10B-O9B
 2.37 with sigma of 0.005
 O8B-O10B
 2.37 with sigma of 0.005
 Cl1A-O10A \\sim Cl1B-O8B \\sim Cl1A-O8A \\sim Cl1B-O9B \\sim Cl1B-O10B \\sim
Cl1A-O9A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1B \\sim O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl1A, Cl1B, O8A, O8B, O9A, O9B, O10A, O10B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=1-FVAR(1)
 Sof(Cl1A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=FVAR(1)
6.a Rotating group:
 O7(H7A)
6.b 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.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_shelx_hkl_checksum              25202
_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 2.065
_oxdiff_exptl_absorpt_empirical_full_min 0.650