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_4127541
_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 H45 N8 Ni4 O14, Cl O4, 11(H2 O)'
_chemical_formula_sum            'C50 H67 Cl N8 Ni4 O29'
_chemical_formula_weight         1514.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.2261(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0432(2)
_cell_length_b                   24.3255(4)
_cell_length_c                   21.4471(4)
_cell_measurement_reflns_used    27084
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      28.2590
_cell_measurement_theta_min      2.6810
_cell_volume                     6183.27(19)
_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(1)
_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     16.00  42.00   0.50   45.00    --   20.59  60.00-178.69   52
  2  \w    -10.00  95.00   0.50   45.00    --   20.59  60.00-112.51  210
  3  \w      2.00  49.00   0.50   45.00    --   20.59  60.00 139.67   94
  4  \w     -4.00  36.00   0.50   45.00    --   20.59  59.00   5.94   80
  5  \w    -10.00  79.00   0.50   45.00    --   20.59  60.00  52.82  178
  6  \w    -25.00  94.00   0.50   45.00    --   20.59  19.00-150.00  238
  7  \w    -42.00 -17.00   0.50   45.00    --   20.59 -57.00-180.00   50
  8  \w     15.00  41.00   0.50   45.00    --   20.59  60.00 -66.67   52
;
_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      -0.0391156000
_diffrn_orient_matrix_UB_12      -0.0199544000
_diffrn_orient_matrix_UB_13      -0.0146007000
_diffrn_orient_matrix_UB_21      -0.0160147000
_diffrn_orient_matrix_UB_22      0.0177541000
_diffrn_orient_matrix_UB_23      -0.0262854000
_diffrn_orient_matrix_UB_31      0.0423750000
_diffrn_orient_matrix_UB_32      -0.0116976000
_diffrn_orient_matrix_UB_33      -0.0149997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76359
_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         28.282
_diffrn_reflns_theta_min         2.275
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.649
_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            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.199
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         15336
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0546P)^2^+12.0939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13381
_reflns_number_total             15336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891382(2-u-OAc-Ni-clo4final)
_cod_original_cell_volume        6183.3(2)
_cod_database_code               4127541
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni4 C50 H67 O29 N8 Cl1 '
_reflns_odcompleteness_completeness 99.90
_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
 O29-O27A
 2.25 with sigma of 0.005
 O28A-O27A
 2.25 with sigma of 0.005
 O27A-O26A
 2.25 with sigma of 0.005
 Cl1A-O26A \\sim Cl1A-O29 \\sim Cl1A-O28A \\sim Cl1A-O27A \\sim Cl1B-O27B \\sim
Cl1B-O26B \\sim Cl1B-
 O28B \\sim Cl1B-O29
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O26B \\sim O28B \\sim O28A \\sim Cl1A \\sim Cl1B \\sim O27B \\sim O27A \\sim
O26A \\sim O29: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4. Rigid body (RIGU) restrains
 O28B, O26B, Cl1B, Cl1A, O28A, O26A, O27B, O29, O27A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1A)=Sof(O26A)=Sof(O28A)=Sof(O27A)=1-FVAR(1)
 Sof(Cl1B)=Sof(O26B)=Sof(O27B)=Sof(O28B)=FVAR(1)
6.a Free rotating group:
 O15(H15a,H15b), O17(H17a,H17b), O25(H25a,H25b), O16(H16a,H16b), O18(H18a,
 H18b), O22(H22a,H22b), O21(H21a,H21b), O23(H23a,H23b), O19(H19a,H19b),
 O20(H20a,H20b), O24(H24a,H24b)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C43(H43), C32(H32), C44(H44), C41(H41), C30(H30), C4(H4), C8(H8a),
 C19(H19), C34(H34), C11(H11), C15(H15), C42(H42), C31(H31), C33(H33), C23(H23),
  C25(H25), C22(H22), C3(H3), C37(H37), C14(H14), C9(H9), C1(H1), C21(H21),
 C24(H24), C10(H10), C35(H35), C13(H13), C2(H2), C20(H20), C12(H12), C36(H36)
6.c Idealised Me refined as rotating group:
 C50(H50a,H50b,H50c), C46(H46a,H46b,H46c), C48(H48a,H48b,H48c)
6.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O5(H5), O7(H7), O8(H8)
;
_shelx_hkl_checksum              12754
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.793