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_7224375
_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
'C94.4 H115.4 Cu4 Na4 O29.2 Si12, 0.6(C2 H6 O)'
_chemical_formula_sum            'C95.6 H119 Cu4 Na4 O29.8 Si12'
_chemical_formula_weight         2428.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-21
_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                90
_cell_angle_beta                 113.730(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6412(9)
_cell_length_b                   19.7915(7)
_cell_length_c                   27.4630(10)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.581
_cell_measurement_theta_min      3.024
_cell_volume                     12261.0(8)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_laue_measured_fraction_full 0.928
_diffrn_reflns_laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49439
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.996
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.604
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1639 before and 0.0830 after correction.
The Ratio of minimum to maximum transmission is 0.6797.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5036
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10296
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0883
_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^)+(0.1478P)^2^+131.9086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             10296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26414f2.cif
_cod_data_source_block           aatol
_cod_original_cell_volume        12260.9(8)
_cod_original_formula_sum        'C95.60 H119 Cu4 Na4 O29.80 Si12'
_cod_database_code               7224375
_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
2. Restrained distances
 O5S-H5S
 0.87 with sigma of 0.01
 C1S-C2S
 1.52 with sigma of 0.01
 O1S-C1S
 1.4 with sigma of 0.01
 O8S-H8S
 0.87 with sigma of 0.01
 O8S-C10S
 2.2 with sigma of 0.01
 O3S-H3S
 0.87 with sigma of 0.01
 O2S-H2S
 0.87 with sigma of 0.01
 C12S-C11S
 1.52 with sigma of 0.01
 C6S-C5S
 1.52 with sigma of 0.01
 Na4-H5S
 2.918979 with sigma of 0.02
 C9S-H8S
 1.910352 with sigma of 0.02
 Na4-H8S
 3.225358 with sigma of 0.02
 C5S-H3S
 1.890285 with sigma of 0.02
 Na4-H3S
 2.749582 with sigma of 0.02
 C11S-H5S
 1.882849 with sigma of 0.02
 C3S-H2S
 1.886573 with sigma of 0.02
 Na2-H2S
 3.167551 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7S) = Uanis(O8S)
4. Rigid body (RIGU) restrains
 Na1, C1S, O1S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Na4, C7S, C8S, O7S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3S, C6S, C5S, O4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Na2, O2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Na4(0.6) Na2(0.5) Na3(0.4) Na1(0.5) O5S(0.5) H5S(0.5) C1S(0.5)
 H1SA(0.5) H1SB(0.5) O1S(0.5) H1S(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5)
 O2S(0.5) H2S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
 H4SC(0.5) O3S(0.3) H3S(0.3) C6S(0.6) H6SA(0.6) H6SB(0.6) H6SC(0.6) C5S(0.6)
 H5SA(0.3) H5SB(0.3) H5SC(0.3) H5SD(0.3) O4S(0.3) H4S(0.4) C7S(0.3) H7SA(0.3)
 H7SB(0.3) C8S(0.3) H8SA(0.3) H8SB(0.3) H8SC(0.3) O7S(0.3) H7S(0.3) C11S(0.7)
 H11A(0.5) H11B(0.5) H11C(0.2) H11D(0.2) C12S(0.7) H12A(0.7) H12B(0.7)
 H12C(0.7) O8S(0.3) H8S(0.3) O6S(0.2) H6S(0.2) C10S(0.3) H10A(0.3) H10B(0.3)
 H10C(0.3) C9S(0.3) H9SA(0.3) H9SB(0.3)
6.a Riding coordinates:
 O1S(H1S), O2S(H2S), O3S(H3S), O4S(H4S), O7S(H7S), O8S(H8S), O6S(H6S)
6.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C3S(H3SA,H3SB), C5S(H5SA,H5SB), C5S(H5SC,H5SD), C7S(H7SA,
 H7SB), C11S(H11A,H11B), C11S(H11C,H11D), C9S(H9SA,H9SB)
6.c Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C4S(H4SA,H4SB,H4SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,H8SB,
 H8SC), C12S(H12A,H12B,H12C), C10S(H10A,H10B,H10C)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C16(H16), C20(H20), C34(H34), C5(H5), C23(H23), C6(H6), C19(H19),
 C17(H17), C30(H30), C40(H40), C38(H38), C31(H31), C41(H41), C33(H33), C3(H3),
 C10(H10), C12(H12), C27(H27), C37(H37), C24(H24), C13(H13), C2(H2), C26(H26)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C42(H42A,H42B,H42C), C7(H7A,H7B,H7C), C35(H35A,H35B,
 H35C), C21(H21A,H21B,H21C), C2S(H2SA,H2SB,H2SC)
;
_olex2_submission_special_instructions 'No special instructions were received'