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_4127537
_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         'C46 H45 N8 Ni4 O13, 3(H2 O), O, 3(N O3)'
_chemical_formula_sum            'C46 H53 N11 Ni4 O26'
_chemical_formula_weight         1410.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                91.475(2)
_cell_angle_beta                 100.300(2)
_cell_angle_gamma                91.778(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7709(3)
_cell_length_b                   13.3769(3)
_cell_length_c                   17.3977(4)
_cell_measurement_reflns_used    14317
_cell_measurement_temperature    183.1(3)
_cell_measurement_theta_max      69.9480
_cell_measurement_theta_min      3.3010
_cell_volume                     2692.60(11)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  20.00   0.50    6.00    --  -51.91  57.00  30.00  172
  2  \w    -61.00  25.00   0.50    6.00    --  -51.91  38.00-156.00  172
  3  \w    -77.00  -9.00   0.50   20.00    --  -84.25  45.00 -30.00  136
  4  \w    -86.00 -29.00   0.50   20.00    --  -84.25 111.00 120.00  114
  5  \w   -106.00 -11.00   0.50   20.00    --  -84.25  77.00  90.00  190
  6  \w   -129.00 -43.00   0.50    6.00    --  -51.91 -38.00 -30.00  172
  7  \w   -126.00 -70.00   0.50    6.00    --  -51.91-125.00-150.00  112
  8  \w   -127.00 -82.00   0.50    6.00    --  -51.91 -99.00 -90.00   90
  9  \w   -129.00 -43.00   0.50    6.00    --  -51.91 -38.00-120.00  172
 10  \w   -127.00 -82.00   0.50    6.00    --  -51.91 -99.00  30.00   90
 11  \w   -127.00 -82.00   0.50    6.00    --  -51.91 -99.00 120.00   90
 12  \w   -127.00 -82.00   0.50    6.00    --  -51.91 -99.00 150.00   90
 13  \w     30.00 109.00   0.50   20.00    --  105.75 -94.00 -30.00  158
 14  \w     88.00 116.00   0.50   20.00    --  105.75 -15.00   0.00   56
 15  \w     96.00 178.00   0.50   20.00    --  105.75  15.00 -90.00  164
 16  \w     96.00 178.00   0.50   20.00    --  105.75  15.00-180.00  164
 17  \w    106.00 164.00   0.50   20.00    --  105.75  15.00-120.00  116
 18  \w     62.00 103.00   0.50   20.00    --  105.75-111.00-180.00   82
 19  \w     33.00  68.00   0.50   20.00    --  105.75 -94.00 -60.00   70
 20  \w     42.00 100.00   0.50   20.00    --  105.75 -94.00-120.00  116
 21  \w     45.00  70.00   0.50   20.00    --  105.75 -45.00-150.00   50
 22  \w     35.00  62.00   0.50   20.00    --  105.75 -30.00-150.00   54
 23  \w     30.00  77.00   0.50   20.00    --  105.75 -45.00 -60.00   94
 24  \w     29.00 112.00   0.50   20.00    --  105.75-111.00-120.00  166
 25  \w     29.00 112.00   0.50   20.00    --  105.75-111.00 -30.00  166
 26  \w     44.00 100.00   0.50   20.00    --  105.75 -77.00  60.00  112
 27  \w     55.00  96.00   0.50   20.00    --  105.75-111.00 150.00   82
 28  \w     30.00  77.00   0.50   20.00    --  105.75 -45.00 120.00   94
 29  \w     38.00  63.00   0.50   20.00    --  105.75 -30.00 120.00   50
 30  \w     28.00  60.00   0.50   20.00    --  105.75 -30.00  90.00   64
 31  \w     29.00  64.00   0.50   20.00    --  105.75 -30.00  60.00   70
 32  \w     26.00  75.00   0.50   20.00    --  105.75 -15.00   0.00   98
 33  \w     28.00  54.00   0.50   20.00    --  105.75 -30.00 -30.00   52
 34  \w     28.00  65.00   0.50   20.00    --  105.75 -30.00 -60.00   74
 35  \w     34.00 112.00   0.50   20.00    --  105.75-111.00  60.00  156
 36  \w     30.00 107.50   0.50   20.00    --  105.75 -94.00  60.00  155
 37  \w     31.00  68.00   0.50   20.00    --  105.75 -30.00 150.00   74
 38  \w    106.00 146.00   0.50   20.00    --  105.75 178.00  90.00   80
;
_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      0.0935420000
_diffrn_orient_matrix_UB_12      0.0691891000
_diffrn_orient_matrix_UB_13      -0.0244012000
_diffrn_orient_matrix_UB_21      0.0936644000
_diffrn_orient_matrix_UB_22      -0.0717942000
_diffrn_orient_matrix_UB_23      0.0355809000
_diffrn_orient_matrix_UB_31      -0.0139716000
_diffrn_orient_matrix_UB_32      -0.0578609000
_diffrn_orient_matrix_UB_33      -0.0790366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41551
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98320
_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 greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       prism
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0324P)^2^+1.7961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7990
_reflns_number_total             10220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891361(2(halfgem-aqua)-Ni4-NO3final)
_cod_original_cell_volume        2692.59(12)
_cod_database_code               4127537
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C46 H49 N13 Ni4 O24'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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
 O13-H13b
 0.85 with sigma of 0.02
3.a Free rotating group:
 O14(H14a,H14b), O15(H15a,H15b), O17(H17a,H17b)
3.b Rotating group:
 O9(H9a,H9b), O10(H10a,H10b), O13(H13a)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8a), C9(H9), C10(H10), C11(H11), C12(H12),
  C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C41(H41), C42(H42), C43(H43), C44(H44)
3.d Idealised Me refined as rotating group:
 C46(H46a,H46b,H46c)
3.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8)
;
_shelx_hkl_checksum              22863
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.911