Dimer formation upon deprotonation: synthesis and structure of a m-terphenyl substituted (R,S)-dilithium disiloxanolate disilanol.
Čas, Daniel; Hurkes, Natascha; Spirk, Stefan; Belaj, Ferdinand; Bruhn, Clemens; Rechberger, Gerald N.; Pietschnig, Rudolf; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12818–12823; doi:10.1039/c5dt01992c

data_7035424
_publ_section_title
;
 Dimer formation upon deprotonation: synthesis and structure of a
 m-terphenyl substituted (R,S)-dilithium disiloxanolate disilanol.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12818
_journal_page_last               12823
_journal_paper_doi               10.1039/c5dt01992c
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         '0.9488(C48 H54 O5 Si2), 0.1024(C24 H25 I)'
_chemical_formula_sum            'C48 H53.7952 I0.1024 O4.744 Si1.8976'
_chemical_formula_weight         772.91
_chemical_name_common
1,3-bis(2,2'',4,4'',6,6''-hexamethyl[1,1':3',1''-ter-phenyl]-2'-yl)-1,1,3,3-disiloxanetetrol
_chemical_name_systematic
1,3-bis(2,2'',4,4'',6,6''-hexamethyl[1,1':3',1''-ter-phenyl]-2'-yl)-1,1,3,3-disiloxanetetrol
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2015-04-15 deposited with the CCDC.
2015-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0956(3)
_cell_length_b                   36.8415(11)
_cell_length_c                   12.6169(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.14
_cell_volume                     4136.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37642
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             1647
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         9822
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0225P)^2^+3.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8179
_reflns_number_total             9822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01992c2.cif
_cod_data_source_block           S69
_cod_depositor_comments
'Adding full bibliography for 7035423--7035427.cif.'
_cod_database_code               7035424
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.941
_exptl_absorpt_special_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_shelxl_version_number           2014/6
_shelx_res_checksum              70987