Synthesis and structure of new polyhedral Ni, Na- and Cu, Na-metallasiloxanes with tolyl substituent at the silicon atom
Anisimov, Anton A.; Kononevich, Yuriy N.; Zhemchugov, Pavel V.; Milenin, Sergey A.; Korlyukov, Alexander A.; Tsareva, Ul'yana S.; Peregudov, Alexander S.; Dorovatovskii, Pavel V.; Molodtsova, Yuliya A.; Takazova, Rina U.; Shchegolikhina, Olga I.; Muzafarov, Aziz M.; RSC Adv. 6 (2016) 22052–; doi:10.1039/C5RA26414F

data_7224373
_publ_section_title
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 Synthesis and structure of new polyhedral Ni, Na- and Cu,
 Na-metallasiloxanes with tolyl substituent at the silicon atom
;
_journal_issue                   26
_journal_name_full               'RSC Adv.'
_journal_page_first              22052
_journal_paper_doi               10.1039/C5RA26414F
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C108 H162 Na6 Ni4 O40 Si12, 2(C2 H6 O)'
_chemical_formula_sum            'C112 H174 Na6 Ni4 O42 Si12'
_chemical_formula_weight         2902.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-12 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                113.9140(10)
_cell_angle_beta                 96.9800(10)
_cell_angle_gamma                95.989(2)
_cell_formula_units_Z            1
_cell_length_a                   14.7272(4)
_cell_length_b                   15.6359(4)
_cell_length_c                   16.9320(5)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.79
_cell_measurement_theta_min      3.25
_cell_volume                     3486.80(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_laue_measured_fraction_full 0.926
_diffrn_reflns_laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43689
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.991
_diffrn_reflns_theta_min         3.249
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.423
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1251 before and 0.0432 after correction.
The Ratio of minimum to maximum transmission is 0.8493.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.032
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         11698
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1218P)^2^+10.6086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10439
_reflns_number_total             11698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26414f2.cif
_cod_data_source_block           pg1042
_cod_database_code               7224373
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O18-C46
 1.42 with sigma of 0.005
 C49-C48
 1.52 with sigma of 0.005
 C47-C46
 1.52 with sigma of 0.005
 O18-H18
 0.85 with sigma of 0.01
 O19-H19
 0.85 with sigma of 0.01
 C58-C57
 1.52 with sigma of 0.005
 O22-H22
 0.85 with sigma of 0.01
 C024-C0 = C029-C024
 1.52 with sigma of 0.005
 O17-C48
 1.42 with sigma of 0.005
 O17-H17
 0.85 with sigma of 0.01
 O21-H21
 0.85 with sigma of 0.01
 C56-C55
 1.55 with sigma of 0.005
 C54-C53
 1.55 with sigma of 0.005
 O15-C55 = O15-C53
 1.42 with sigma of 0.005
 O15-H15A
 0.87 with sigma of 0.01
 O15-H15
 0.87 with sigma of 0.01
 C46-H18
 1.8821 with sigma of 0.02
 Na3-H18
 2.614804 with sigma of 0.02
 C43-H19
 1.894733 with sigma of 0.02
 Na3-H19
 2.714537 with sigma of 0.02
 Na1-H22
 3.130704 with sigma of 0.02
 C024-H22
 1.858297 with sigma of 0.02
 C48-H17
 1.881537 with sigma of 0.02
 Na3-H17
 2.51026 with sigma of 0.02
 C01P-H21
 1.8634 with sigma of 0.02
 Na1-H21
 2.798025 with sigma of 0.02
 C53-H15A
 1.900958 with sigma of 0.02
 Na2-H15A
 2.667402 with sigma of 0.02
 C55-H15
 1.896965 with sigma of 0.02
 Na2-H15
 2.988916 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53 \\sim C55: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C0 \\sim C029: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C54 \\sim C56: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uiso(C48) = Uiso(C46)
Uiso(C49) = Uiso(C47)
Uiso(O17) = Uiso(O18)
4. Others
 Sof(O18)=Sof(H18)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=1-FVAR(1)
 Sof(O17)=Sof(H17)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=
 Sof(H49C)=FVAR(1)
 Fixed Sof: H15A(0.5) H15(0.5) C0(0.13725) H0A(0.13725) H0B(0.13725)
 H0C(0.13725) C029(0.86275) H02C(0.86275) H02D(0.86275) H02E(0.86275)
 H43C(0.75) H43D(0.75) H43A(0.25) H43B(0.25) C44(0.25) H44A(0.25) H44B(0.25)
 H44C(0.25) C45(0.75) H45A(0.75) H45B(0.75) H45C(0.75) C53(0.5) H53A(0.5)
 H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) H57A(0.5) H57B(0.5) H57C(0.5) H57D(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 H50A(0.75) H50B(0.75) H50C(0.25) H50D(0.25) C51(0.25) H51A(0.25) H51B(0.25)
 H51C(0.25) C52(0.75) H52A(0.75) H52B(0.75) H52C(0.75)
 Fixed Uiso: C55(0.09367) C56(0.12)
5.a Riding coordinates:
 O0(H0), O13(H13A,H13B), O14(H14), O15(H15A), O15(H15), O17(H17), O21(H21),
 O16(H16A)
5.b Secondary CH2 refined with riding coordinates:
 C01P(H01A,H01B), C024(H02A,H02B), C43(H43C,H43D), C43(H43A,H43B), C46(H46A,
 H46B), C48(H48A,H48B), C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B),
 C57(H57C,H57D), C50(H50A,H50B), C50(H50C,H50D)
5.c Me refined with riding coordinates:
 C0(H0A,H0B,H0C), C029(H02C,H02D,H02E), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17A), C19(H19A), C20(H20), C23(H23), C24(H24), C26(H26),
 C27(H27), C30(H30), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C40(H40),
  C41(H41)
5.e Idealised Me refined as rotating group:
 C01W(H01C,H01D,H01E), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'