Unusual penta- and hexanuclear Ni(ii)-based silsesquioxane polynuclear complexes.
Bilyachenko, Alexey N.; Yalymov, Alexey I.; Korlyukov, Alexander A.; Long, Jérôme; Larionova, Joulia; Guari, Yannick; Vologzhanina, Anna V.; Es'kova, Marina A.; Shubina, Elena S.; Levitsky, Mikhail M.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7320–7327; doi:10.1039/c6dt00113k

data_7038758
_publ_section_title
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 Unusual penta- and hexanuclear Ni(ii)-based silsesquioxane polynuclear
 complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7320
_journal_page_last               7327
_journal_paper_doi               10.1039/c6dt00113k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C102 H102 Cl N2 Ni6 O32 Si12, C16 H29 Na O10, 5(C4 H8 O2)'
_chemical_formula_sum            'C138 H171 Cl N2 Na Ni6 O52 Si12'
_chemical_formula_weight         3437.54
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2016-01-10 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.513(2)
_cell_angle_gamma                90.00
_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_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  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_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_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_theta_full        30.18
_diffrn_reflns_theta_max         30.18
_diffrn_reflns_theta_min         1.36
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3586
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.538
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         23101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+2.4130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.2105
_reflns_number_gt                11161
_reflns_number_total             23101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00113k2.cif
_cod_data_source_block           ses50
_cod_depositor_comments
;
Adding full bibliography for 7038757--7038758.cif.

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
'C51 H51 Cl0.5 N Ni3 O16 Si6, C8 H14.5 Na0.5 O5, 2.5(C4 H8 O2)'
_cod_original_formula_sum        'C69 H85.50 Cl0.50 N Na0.50 Ni3 O26 Si6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1718.77
_cod_database_code               7038758
_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) H58(0.5) C57(0.5) H57(0.5) C60(0.5) H60(0.5) C59(0.5)
 H59(0.5) C70(0.5) H70A(0.5) H70B(0.5) C69(0.5) H69(0.5) C67(0.5) H67(0.5)
 C68(0.5) H68(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,C78,C88,C87), O25(O23,C80,C79,C89,C90)
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), C70(H70A,H70B),
 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), C58(H58), C57(H57), C60(H60), C59(H59),
 C69(H69), C67(H67), C68(H68)
;