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_7038757
_publ_section_title
;
 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         'C81 H100 N7 Na Ni5 O28 Si10'
_chemical_formula_sum            'C81 H100 N7 Na Ni5 O28 Si10'
_chemical_formula_weight         2217.11
_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             2016-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-10 deposited with the CCDC.
2016-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.703(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1408(17)
_cell_length_b                   18.6886(16)
_cell_length_c                   27.306(2)
_cell_measurement_reflns_used    9591
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.30
_cell_volume                     10266.6(14)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            133509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.521
_diffrn_reflns_theta_min         1.012
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.8286.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4600
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.716
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         31342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0656P)^2^+7.5096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23643
_reflns_number_total             31342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00113k2.cif
_cod_data_source_block           paa76
_cod_depositor_comments
'Adding full bibliography for 7038757--7038758.cif.'
_cod_original_cell_volume        10266.8(15)
_cod_database_code               7038757
_shelxl_version_number           2014/6
_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, All O(H) groups
2.a Riding coordinates:
 O100(H100)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C9(H9), C16(H16), C37(H37), C96(H96), C92(H92), C93(H93), C86(H86),
 C47(H47), C19(H19), C46(H46), C95(H95), C94(H94), C42(H42), C76(H76),
 C106(H106), C45(H45), C85(H85), C102(H102), C12(H12), C43(H43), C75(H75),
 C74(H74), C66(H66), C36(H36), C6(H6), C44(H44), C65(H65), C3(H3), C15(H15),
 C62(H62), C26(H26), C82(H82), C103(H103), C104(H104), C72(H72), C22(H22),
 C13(H13), C105(H105), C84(H84), C35(H35), C24(H24), C14(H14), C34(H34),
 C25(H25), C32(H32), C63(H63), C54(H54), C64(H64), C23(H23), C52(H52), C83(H83),
  C56(H56), C73(H73), C55(H55), C33(H33), C53(H53)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C),
 C29(H29A,H29B,H29C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C),
  C39(H39A,H39B,H39C), C5(H5A,H5B,H5C), C49(H49A,H49B,H49C), C4(H4A,H4B,H4C),
 C17(H17A,H17B,H17C), C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'