A Hexagonal Ni6 Cluster Protected by 2-Phenylethanethiol for Catalytic Conversion of Toluene to Benzaldehyde
Pembere, Anthony M.; Cui, Chaonan; Anumula, Rajini; Wu, Huiming; An, Pan; Liang, Tongling; Luo, Zhixun; Physical Chemistry Chemical Physics  (2019) –; doi:10.1039/C9CP02964H

data_7233235
_publ_section_title
;
 A Hexagonal Ni6 Cluster Protected by 2-Phenylethanethiol for Catalytic
 Conversion of Toluene to Benzaldehyde
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/C9CP02964H
_journal_year                    2019
_chemical_formula_moiety         'C96 H108 Ni6 S12'
_chemical_formula_sum            'C96 H108 Ni6 S12'
_chemical_formula_weight         1998.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 92.071(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.244(3)
_cell_length_b                   12.415(3)
_cell_length_c                   32.461(9)
_cell_measurement_reflns_used    14461
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      1.2554
_cell_volume                     4528(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            32180
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         1.939
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0089P)^2^+8.5062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9319
_reflns_number_total             10290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp02964h1.cif
_cod_data_source_block           mx7095l
_cod_database_code               7233235
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B),
 C24(H24A,H24B), C31(H31A,H31B), C32(H32A,H32B), C39(H39A,H39B), C40(H40A,H40B),
  C47(H47A,H47B), C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              60227
_shelx_hkl_checksum              9679
_olex2_submission_special_instructions 'No special instructions were received'