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_4127522
_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         'C38 H32 Co2 N4 O6, H2 O, C2 H3 N'
_chemical_formula_sum            'C40 H37 Co2 N5 O7'
_chemical_formula_weight         817.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 95.987(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2864(2)
_cell_length_b                   21.6644(5)
_cell_length_c                   18.8463(5)
_cell_measurement_reflns_used    23377
_cell_measurement_temperature    182.9(7)
_cell_measurement_theta_max      28.9710
_cell_measurement_theta_min      2.4530
_cell_volume                     3770.90(16)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      182.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_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    -17.00  86.00   1.00   90.00    --   12.18  57.00-150.00  103
  2  \w    -18.00  86.00   1.00   90.00    --   12.18  60.00  33.23  104
  3  \w    -18.00  86.00   1.00   90.00    --   12.18  58.00 178.66  104
  4  \w    -18.00  86.00   1.00   90.00    --   12.18  59.00 -46.12  104
  5  \w    -62.00  42.00   1.00   90.00    --   12.18 -57.00  30.00  104
  6  \w    -41.00  63.00   1.00   90.00    --  -11.40  57.00 150.00  104
  7  \w    -62.00  -4.00   1.00   90.00    --   12.18 -58.00 -50.03   58
  8  \w    -62.00  42.00   1.00   90.00    --   12.18 -57.00-120.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0466921000
_diffrn_orient_matrix_UB_12      0.0223111000
_diffrn_orient_matrix_UB_13      -0.0129317000
_diffrn_orient_matrix_UB_21      0.0369963000
_diffrn_orient_matrix_UB_22      -0.0237152000
_diffrn_orient_matrix_UB_23      -0.0166759000
_diffrn_orient_matrix_UB_31      -0.0484486000
_diffrn_orient_matrix_UB_32      0.0033848000
_diffrn_orient_matrix_UB_33      -0.0314237000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76910
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.355
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.791
_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    1.440
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         7715
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0305P)^2^+3.4711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6675
_reflns_number_total             7715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891333(Co-dp(Ph)OHdimer)
_cod_database_code               4127522
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H34 Co2 N4 O7'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 N5A-C40A
 1.17 with sigma of 0.005
 N5B-C40B
 1.17 with sigma of 0.005
 C39B-C40B
 1.46 with sigma of 0.005
 C39B-N5B
 2.63 with sigma of 0.005
 C39A-N5A
 2.63 with sigma of 0.005
 N5B-C40B \\sim N5A-C40A
 with sigma of 0.005
 C39B-C40B \\sim C39A-C40A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N5A \\sim N5B \\sim C39A \\sim C39B \\sim C40A \\sim C40B: within 2A with sigma
of 0.002 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N5A, N5B, C39A, C39B, C40A, C40B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N5B)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40B)=1-FVAR(1)
 Sof(N5A)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40A)=FVAR(1)
6.a Free rotating group:
 O7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
 C33(H33), C34(H34)
6.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39A(H39A,H39B,H39C), C39B(H39D,
 H39E,H39F)
;
_shelx_hkl_checksum              50902
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.823