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_4127538
_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, B F4, 2.75(H2 O), 8.25(O)'
_chemical_formula_sum            'C50 H67 B F4 N8 Ni4 O25'
_chemical_formula_weight         1501.76
_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                 101.629(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9815(3)
_cell_length_b                   24.6554(7)
_cell_length_c                   21.5499(6)
_cell_measurement_reflns_used    20284
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      27.5760
_cell_measurement_theta_min      2.4520
_cell_volume                     6235.4(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -27.00  37.00   0.50  100.00    --    3.92 -99.00  30.00  128
  2  \w     35.00  83.00   0.50  100.00    --    3.92-178.00-120.00   96
  3  \w    -27.00  29.00   0.50  100.00    --   -4.86 -99.00-150.00  112
  4  \w     -6.00  72.00   0.50  100.00    --   -4.86  38.00-120.00  156
  5  \w    -20.00  24.00   0.50  100.00    --   -4.86  57.00   0.00   88
  6  \w     38.00  50.00   0.50  100.00    --    3.92 178.00  30.00   24
;
_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      -0.0357566000
_diffrn_orient_matrix_UB_12      -0.0193638000
_diffrn_orient_matrix_UB_13      -0.0186239000
_diffrn_orient_matrix_UB_21      -0.0146849000
_diffrn_orient_matrix_UB_22      0.0194011000
_diffrn_orient_matrix_UB_23      -0.0245918000
_diffrn_orient_matrix_UB_31      0.0464795000
_diffrn_orient_matrix_UB_32      -0.0087783000
_diffrn_orient_matrix_UB_33      -0.0132763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (Rigaku Oxford Diffraction, 2015)
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    1.600
_exptl_crystal_description       prism
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         14218
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0517P)^2^+9.0542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11810
_reflns_number_total             14218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01356_si_002.cif
_cod_data_source_block           1891379(2-u-OAc-ni4-bf4final)
_cod_database_code               4127538
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C228 H260 B4 F8 N52 Ni16 O56 '
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.671
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H18A(0.075) H18B(0.075) H29A(0.074) H29B(0.074) H1(0.029)
 H2(0.037) H3(0.04) H4(0.033) H8A(0.033) H9(0.044) H10(0.045) H11(0.035)
 H12(0.034) H13(0.042) H14(0.043) H15(0.034) H19(0.037) H20(0.046) H21(0.043)
 H22(0.033) H23(0.03) H24(0.038) H25(0.041) H26(0.033) H30(0.033) H31(0.04)
 H32(0.038) H33(0.031) H34(0.029) H35(0.034) H36(0.032) H37(0.025) H41(0.028)
 H42(0.041) H43(0.047) H44(0.034) H46A(0.068) H46B(0.068) H46C(0.068)
 H48A(0.073) H48B(0.073) H48C(0.073) H50A(0.042) H50B(0.042) H50C(0.042)
 Fixed X: H5(-0.63993) H6(-0.555886) H7(-0.95468) H8(-0.415202) H15A(-
 0.245903) H15B(-0.327104) H18A(-0.349808) H18B(-0.451349) H29A(-0.728953)
 H29B(-0.765601) H1(-0.266683) H2(-0.155646) H3(-0.235234) H4(-0.425312) H8A(-
 0.618618) H9(-0.749187) H10(-0.859509) H11(-0.830295) H12(-1.001682) H13(-
 1.105688) H14(-1.02518) H15(-0.839795) H19(-0.628853) H20(-0.584261) H21(-
 0.58882) H22(-0.643501) H23(-0.703366) H24(-0.836462) H25(-1.008544) H26(-
 1.045008) H30(-1.134367) H31(-1.211461) H32(-1.089194) H33(-0.893506) H34(-
 0.537305) H35(-0.372085) H36(-0.272429) H37(-0.339446) H41(-0.511454) H42(-
 0.64195) H43(-0.813935) H44(-0.851916) H46A(-0.238933) H46B(-0.335491) H46C(-
 0.251086) H48A(-1.033583) H48B(-1.009678) H48C(-0.954522) H50A(-0.541067)
 H50B(-0.581419) H50C(-0.454177)
 Fixed Y: H5(-0.614294) H6(-0.808821) H7(-0.713011) H8(-0.85904) H15A(-
 0.693542) H15B(-0.731202) H18A(-0.54799) H18B(-0.576598) H29A(-0.481485) H29B(-
 0.517016) H1(-0.759849) H2(-0.704115) H3(-0.624055) H4(-0.602381) H8A(-
 0.554553) H9(-0.52269) H10(-0.585675) H11(-0.677531) H12(-0.723878) H13(-
 0.772745) H14(-0.850484) H15(-0.876623) H19(-0.906404) H20(-0.997232) H21(-
 1.028248) H22(-0.968967) H23(-0.784315) H24(-0.828794) H25(-0.857672) H26(-
 0.838073) H30(-0.80432) H31(-0.873689) H32(-0.936778) H33(-0.929097) H34(-
 0.690922) H35(-0.706957) H36(-0.788106) H37(-0.850621) H41(-0.908324) H42(-
 0.972961) H43(-0.985772) H44(-0.934341) H46A(-0.886807) H46B(-0.929283) H46C(-
 0.90499) H48A(-0.587577) H48B(-0.612863) H48C(-0.555813) H50A(-0.670046) H50B(-
 0.619047) H50C(-0.64163)
 Fixed Z: H5(-0.479866) H6(-0.340079) H7(-0.585311) H8(-0.518492) H15A(-
 0.329796) H15B(-0.348302) H18A(-0.448412) H18B(-0.44488) H29A(-0.452397) H29B(-
 0.501486) H1(-0.490606) H2(-0.541087) H3(-0.59023) H4(-0.58722) H8A(-0.576093)
 H9(-0.664952) H10(-0.733267) H11(-0.714755) H12(-0.442316) H13(-0.381258) H14(-
 0.32788) H15(-0.335486) H19(-0.310064) H20(-0.32625) H21(-0.429547) H22(-
 0.513593) H23(-0.751734) H24(-0.828379) H25(-0.802911) H26(-0.702166) H30(-
 0.601018) H31(-0.547707) H32(-0.487322) H33(-0.481622) H34(-0.70016) H35(-
 0.738379) H36(-0.71132) H37(-0.644836) H41(-0.691917) H42(-0.743857) H43(-
 0.709702) H44(-0.626053) H46A(-0.418483) H46B(-0.409603) H46C(-0.348864) H48A(-
 0.52381) H48B(-0.588275) H48C(-0.563326) H50A(-0.279291) H50B(-0.324155) H50C(-
 0.316657)
;
_shelx_hkl_checksum              30273
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.469