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_4127539
_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, H2 O, 10.5(O)'
_chemical_formula_sum            'C50 H68 Cl N8 Ni4 O25.5'
_chemical_formula_weight         1459.41
_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                 100.333(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9510(3)
_cell_length_b                   24.1715(5)
_cell_length_c                   21.5060(6)
_cell_measurement_reflns_used    21704
_cell_measurement_temperature    183.00(10)
_cell_measurement_theta_max      26.3350
_cell_measurement_theta_min      2.1410
_cell_volume                     6111.8(3)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_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    -15.00  84.00   0.50  100.00    --    3.20  19.00 -30.00  198
  2  \w    -27.00  39.00   0.50  100.00    --    3.20 -99.00 120.00  132
  3  \w    -27.00  32.00   0.50  100.00    --   -4.14 -99.00 -60.00  118
  4  \w    -64.00  20.00   0.50  100.00    --    3.20 -38.00 -60.00  168
  5  \w     38.00  84.00   0.50  100.00    --    3.20 178.00 -60.00   92
;
_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      0.0125254000
_diffrn_orient_matrix_UB_12      -0.0262267000
_diffrn_orient_matrix_UB_13      -0.0118291000
_diffrn_orient_matrix_UB_21      0.0223568000
_diffrn_orient_matrix_UB_22      0.0131419000
_diffrn_orient_matrix_UB_23      -0.0246336000
_diffrn_orient_matrix_UB_31      0.0546144000
_diffrn_orient_matrix_UB_32      0.0006460000
_diffrn_orient_matrix_UB_33      0.0194221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66759
_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         26.373
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_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    1.586
_exptl_crystal_description       prism
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         12486
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0635P)^2^+10.7619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10555
_reflns_number_total             12486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891380(2-u-oac-ni4-clfinal)
_cod_original_formula_sum        'C50 H68 Cl N8 Ni4 O25.50'
_cod_database_code               4127539
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 Cl N8 Ni4 O26'
_reflns_odcompleteness_completeness 99.85
_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
 O6-H6
 0.85 with sigma of 0.02
3. Others
 Sof(O19B)=1-FVAR(1)
 Sof(O19A)=FVAR(1)
 Fixed Sof: Cl1A(0.6) Cl1B(0.4) O17A(0.5) O17B(0.5) O22A(0.5) O22B(0.5)
 O22C(0.5)
4.a Free rotating group:
 O15(H15a,H15b)
4.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C22(H22), C36(H36), C34(H34), C35(H35), C1(H1), C30(H30), C4(H4),
 C19(H19), C23(H23), C11(H11), C44(H44), C26(H26), C12(H12), C43(H43), C15(H15),
  C2(H2), C8(H8a), C42(H42), C33(H33), C24(H24), C25(H25), C21(H21), C41(H41),
 C20(H20), C3(H3), C14(H14), C31(H31), C10(H10), C13(H13), C9(H9), C32(H32)
4.c Idealised Me refined as rotating group:
 C48(H48a,H48b,H48c), C50(H50a,H50b,H50c), C46(H46a,H46b,H46c)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7), O8(H8)
;
_shelx_hkl_checksum              9882
_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 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.590