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_7224376
_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         'C120 H192 O24 Si24, C9 H18'
_chemical_formula_sum            'C129 H210 O24 Si24'
_chemical_formula_weight         2819.12
_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
_audit_creation_date             2015-09-16
_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                71.01(3)
_cell_angle_beta                 88.51(3)
_cell_angle_gamma                62.94(3)
_cell_formula_units_Z            2
_cell_length_a                   18.511(4)
_cell_length_b                   19.755(4)
_cell_length_c                   26.771(5)
_cell_measurement_temperature    120
_cell_volume                     8157(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.778
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.987
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_laue_measured_fraction_full 0.778
_diffrn_reflns_laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            135390
_diffrn_reflns_point_group_measured_fraction_full 0.778
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        36.313
_diffrn_reflns_theta_max         34.605
_diffrn_reflns_theta_min         3.389
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1642
_refine_ls_number_reflns         22936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0978P)^2^+1.2770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17715
_reflns_number_total             22936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26414f2.cif
_cod_data_source_block           aa127
_cod_original_cell_volume        8156(4)
_cod_database_code               7224376
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
 C49(H49), C52(H52), C53(H53), C55(H55), C56(H56), C59(H59), C60(H60), C62(H62),
  C63(H63), C66(H66), C67(H67), C69(H69), C70(H70), C73(H73), C74(H74),
 C76(H76), C77(H77), C83(H83), C84(H84), C86(H86), C87(H87), C96(H96), C97(H97),
  C99(H99), C100(H100), C103(H103), C104(H104), C106(H106), C107(H107),
 C110(H110), C111(H111), C113(H113), C114(H114), C118(H118), C119(H119),
 C121(H121), C122(H122), C125(H125), C126(H126), C127(H127), C128(H128)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C50(H50A,H50B,H50C), C57(H57A,
 H57B,H57C), C64(H64A,H64B,H64C), C71(H71A,H71B,H71C), C78(H78A,H78B,H78C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C88(H88A,H88B,
 H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C101(H10D,H10E,H10F),
 C108(H10G,H10H,H10I), C115(H11D,H11E,H11F), C116(H11G,H11H,H11I), C123(H12D,
 H12E,H12F)
;
_olex2_submission_special_instructions 'No special instructions were received'