Novel Cage-Like Hexanuclear Nickel(II) Silsesquioxane. Synthesis, Structure, and Catalytic Activity in Oxidations with Peroxides.
Bilyachenko, Alexey N.; Yalymov, Alexey I.; Shul'pina, Lidia S.; Mandelli, Dalmo; Korlyukov, Alexander A.; Vologzhanina, Anna V.; Es'kova, Marina A.; Shubina, Elena S.; Levitsky, Mikhail M.; Shul'pin, Georgiy B.; Molecules (Basel, Switzerland) 21 (2016) 665–; doi:10.3390/molecules21050665

data_1543463
_publ_section_title
;
 Novel Cage-Like Hexanuclear Nickel(II) Silsesquioxane. Synthesis,
 Structure, and Catalytic Activity in Oxidations with Peroxides.
;
_journal_issue                   5
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              665
_journal_paper_doi               10.3390/molecules21050665
_journal_volume                  21
_journal_year                    2016
_chemical_formula_moiety
'C102 H102 Cl N2 Ni6 O32 Si12, C16 H36 Na O10, 5(C4 H8 O2)'
_chemical_formula_sum            'C138 H178 Cl N2 Na Ni6 O52 Si12'
_chemical_formula_weight         3444.59
_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   mixed
_audit_creation_date             2016-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.513(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.1899(12)
_cell_length_b                   18.2778(14)
_cell_length_c                   27.093(2)
_cell_measurement_reflns_used    5486
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.657
_cell_measurement_theta_min      2.401
_cell_volume                     7855.9(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1795
_diffrn_reflns_av_unetI/netI     0.1707
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            100379
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.180
_diffrn_reflns_theta_min         1.358
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.3483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8051.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.600
_refine_diff_density_min         -2.575
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         23101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+2.2341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11161
_reflns_number_total             23101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CCDC-1471551-Molecules-129045.cif
_cod_data_source_block           ses50
_cod_database_code               1543463
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: C58(0.5) H58A(0.5) H58B(0.5) C57(0.5) H57A(0.5) H57B(0.5) C60(0.5)
 H60A(0.5) H60B(0.5) C59(0.5) H59A(0.5) H59B(0.5) C70(0.5) H70A(0.5) H70B(0.5)
 C69(0.5) H69A(0.5) H69B(0.5) C67(0.5) H67A(0.5) H67B(0.5) C68(0.5) H68A(0.5)
 H68B(0.5) O22(0.5) O24(0.5) C77(0.5) H77A(0.5) H77B(0.5) C78(0.5) H78A(0.5)
 H78B(0.5) C88(0.5) H88A(0.5) H88B(0.5) C87(0.5) H87A(0.5) H87B(0.5) O25(0.5)
 O23(0.5) C80(0.5) H80A(0.5) H80B(0.5) C79(0.5) H79A(0.5) H79B(0.5) C89(0.5)
 H89A(0.5) H89B(0.5) C90(0.5) H90A(0.5) H90B(0.5)
 Fixed Uiso: C90(0.12)
3.a Free rotating group:
 O22(O24,C77), O25(O23,C80)
3.b Rotating group:
 O28(H28C,H28D)
3.c Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C17(H17A,H17B), C20(H20A,H20B), C18(H18A,H18B), C30(H30A,
 H30B), C28(H28A,H28B), C29(H29A,H29B), C19(H19A,H19B), C37(H37A,H37B),
 C39(H39A,H39B), C50(H50A,H50B), C49(H49A,H49B), C40(H40A,H40B), C38(H38A,H38B),
  C48(H48A,H48B), C47(H47A,H47B), C8(H8A,H8B), C9(H9A,H9B), C58(H58A,H58B),
 C57(H57A,H57B), C60(H60A,H60B), C59(H59A,H59B), C70(H70A,H70B), C69(H69A,H69B),
  C67(H67A,H67B), C68(H68A,H68B), C77(H77A,H77B), C78(H78A,H78B), C88(H88A,
 H88B), C87(H87A,H87B), C80(H80A,H80B), C79(H79A,H79B), C89(H89A,H89B),
 C90(H90A,H90B)
3.d Aromatic/amide H refined with riding coordinates:
 C52(H52), C42(H42), C66(H66), C62(H62), C3(H3), C25(H25), C36(H36), C46(H46),
 C4(H4), C5(H5), C56(H56), C6(H6), C54(H54), C64(H64), C16(H16), C53(H53),
 C7(H7), C23(H23), C43(H43), C55(H55), C45(H45), C26(H26), C44(H44), C32(H32),
 C12(H12), C14(H14), C65(H65), C13(H13), C63(H63), C22(H22), C24(H24), C35(H35),
  C33(H33), C15(H15), C34(H34)
;
_olex2_submission_special_instructions 'No special instructions were received'