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_4127527
_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 Co1.92 N8 Ni2.08 O14, 2(Cl O4)'
_chemical_formula_sum            'C48 H46 Cl2 Co1.94 N8 Ni2.06 O22'
_chemical_formula_weight         1393.09
_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             2018-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.903(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7499(14)
_cell_length_b                   12.1315(6)
_cell_length_c                   21.1640(12)
_cell_measurement_reflns_used    4646
_cell_measurement_temperature    183.05(10)
_cell_measurement_theta_max      28.2620
_cell_measurement_theta_min      3.1550
_cell_volume                     5254.2(6)
_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      183.05(10)
_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    -90.00   5.00   0.50   50.00    --  -19.81 -57.00 150.00  190
  2  \w    -40.00  49.00   0.50   50.00    --  -19.81  57.00 -60.00  178
  3  \w     12.00  45.00   0.50   50.00    --   20.59 -38.00 -60.00   66
;
_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      0.0127327000
_diffrn_orient_matrix_UB_12      -0.0521762000
_diffrn_orient_matrix_UB_13      0.0148071000
_diffrn_orient_matrix_UB_21      -0.0311446000
_diffrn_orient_matrix_UB_22      -0.0156517000
_diffrn_orient_matrix_UB_23      -0.0029670000
_diffrn_orient_matrix_UB_31      -0.0082847000
_diffrn_orient_matrix_UB_32      -0.0212910000
_diffrn_orient_matrix_UB_33      -0.0340442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14532
_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         28.279
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.894
_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 dark purple'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       prism
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.167
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         6520
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0650P)^2^+18.9902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5013
_reflns_number_total             6520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891349(2-coxni4-x-clo4final)
_cod_database_code               4127527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C48 H46 Cl2 Co4 N8 O22'
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.533
_reflns_odcompleteness_completeness 99.85
_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. Shared sites
{Co2, Ni2}
{Co1, Ni1}
3. Restrained distances
 O7-H7A
 0.86 with sigma of 0.02
 O7-H7B
 0.84 with sigma of 0.02
 O5-C23B \\sim O5-C23A
 with sigma of 0.002
 O6A-C23A \\sim O6B-C23B
 with sigma of 0.002
 C24B-C23B \\sim C24A-C23A
 with sigma of 0.002
 Cl1B-O8B \\sim Cl1B-O9B \\sim Cl1A-O11A \\sim Cl1B-O10B \\sim Cl1A-O10A \\sim
Cl1A-O8A \\sim Cl1A-O9A
 \\sim Cl1B-O11B
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
O8A \\sim O8B \\sim O9A \\sim O9B \\sim O10A \\sim O10B \\sim O11A \\sim O11B:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(Co2) = Uanis(Ni2)
Uanis(Co1) = Uanis(Ni1)
5. Rigid body (RIGU) restrains
 O5, O6A, O6B, C23A, C23B, C24A, C24B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 Cl1A, Cl1B, O8A, O8B, O9A, O9B, O10A, O10B, O11A, O11B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Cl1B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=1-FVAR(1)
 Sof(Cl1A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=FVAR(1)
 Sof(O6A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(O6B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(2)
 Fixed Sof: Co1(0.49) Co2(0.47) Ni1(0.51) Ni2(0.53)
7.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)
7.b Idealised Me refined as rotating group:
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F)
7.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_shelx_hkl_checksum              10201
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.759