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_7224374
_publ_section_title
;
 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
'C59.25 H93.75 O12 Si11.75, 0.25(C2.97 H8.9 Si)'
_chemical_formula_sum            'C60 H96 O12 Si12'
_chemical_formula_weight         1346.44
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-14 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                76.2710(11)
_cell_angle_beta                 77.6651(11)
_cell_angle_gamma                74.0613(10)
_cell_formula_units_Z            2
_cell_length_a                   12.9190(6)
_cell_length_b                   13.6750(6)
_cell_length_c                   23.8149(11)
_cell_measurement_reflns_used    5508
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.41
_cell_volume                     3880.0(3)
_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, 2008)'
_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 0.992
_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  0.0745
_diffrn_reflns_av_unetI/netI     0.1293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52519
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.705
_diffrn_reflns_theta_min         0.891
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.9247.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         23917
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0591P)^2^+2.8519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12234
_reflns_number_total             23917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26414f2.cif
_cod_data_source_block           pzh229
_cod_database_code               7224374
_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
2. Uiso/Uaniso restraints and constraints
Uiso(C62) = Uiso(C63)
Uiso(C63) = Uiso(C62)
Uiso(C61) = Uiso(C60)
Uiso(C65) = Uiso(C64)
Uiso(C45) = Uiso(C44)
Uiso(C43) = Uiso(C42)
Uiso(C46) = Uiso(C47)
Uiso(C48A) = Uiso(C48B)
Uiso(C49A) = Uiso(C49B)
Uiso(C50A) = Uiso(C50B)
3. Same fragment restrains
{Si12, C62, C65, C60} sigma for 1-2: 0.02, 1-3: 0.02
as
{Si13, C61, C63, C64}
4. Others
 Sof(Si12)=1-FVAR(1)
 Sof(Si13)=FVAR(1)
 Fixed Sof: C62(0.25) H62A(0.25) H62B(0.25) H62C(0.25) C65(0.25) H65A(0.25)
 H65B(0.25) H65C(0.25) C60(0.25) H60A(0.25) H60B(0.25) H60C(0.25) C61(0.75)
 H61A(0.75) H61B(0.75) H61C(0.75) C63(0.75) H63A(0.75) H63B(0.75) H63C(0.75)
 C64(0.75) H64A(0.75) H64B(0.75) H64C(0.75) C42(0.6) H42A(0.6) H42B(0.6)
 H42C(0.6) C43(0.4) H43A(0.4) H43B(0.4) H43C(0.4) C44(0.6) H44A(0.6) H44B(0.6)
 H44C(0.6) C45(0.4) H45A(0.4) H45B(0.4) H45C(0.4) C46(0.4) H46A(0.4) H46B(0.4)
 H46C(0.4) C47(0.6) H47A(0.6) H47B(0.6) H47C(0.6) C48B(0.5) H48A(0.5) H48B(0.5)
 H48C(0.5) C49B(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50B(0.5) H50A(0.5)
 H50B(0.5) H50C(0.5) C49A(0.5) H49D(0.5) H49E(0.5) H49F(0.5) C48A(0.5)
 H48D(0.5) H48E(0.5) H48F(0.5) C50A(0.5) H50D(0.5) H50E(0.5) H50F(0.5)
5.a Me refined with riding coordinates:
 C48B(H48A,H48B,H48C), C49B(H49A,H49B,H49C), C50B(H50A,H50B,H50C), C49A(H49D,
 H49E,H49F), C48A(H48D,H48E,H48F), C50A(H50D,H50E,H50F)
5.b 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(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C37(H37), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C1AA(H1AA,H1AB,H1AC), C7(H7A,
 H7B,H7C), C14(H14A,H14B,H14C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C)
;
_olex2_submission_special_instructions 'No special instructions were received'