Synthesis of 2,5-Substituted Siloles and Optical Study of Interactions with Mercury(II), Copper(II), and Nickel(II) Cations
Carroll, James B.; Braddock-Wilking, Janet; Organometallics 32 (2013) 1905–; doi:10.1021/om400022f

data_4080481
_publ_section_title
;
 Synthesis of 2,5-Substituted Siloles and Optical Study of Interactions
 with Mercury(II), Copper(II), and Nickel(II) Cations
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1905
_journal_paper_doi               10.1021/om400022f
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H24 N2 Si'
_chemical_formula_sum            'C32 H24 N2 Si'
_chemical_formula_weight         464.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8812(4)
_cell_length_b                   13.8509(3)
_cell_length_c                   19.7703(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.42
_cell_measurement_theta_min      2.33
_cell_volume                     5170.36(19)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            88966
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0594 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.8980.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.585
_exptl_crystal_size_mid          0.555
_exptl_crystal_size_min          0.543
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         8602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+1.9639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                7010
_reflns_number_total             8602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400022f_si_002.cif
_cod_data_source_block           w54211
_cod_database_code               4080481
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H29 of C29, H22 of C22, H12 of C12, H8 of C8, H20 of C20, H26 of C26, H11
  of C11, H27 of C27, H14 of C14, H17 of C17, H21 of C21, H15 of C15, H18 of
  C18, H30 of C30, H9 of C9, H24 of C24, H23 of C23, H16 of C16
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1
2.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C12(H12), C8(H8), C20(H20), C26(H26), C11(H11), C27(H27), C24(H24),
 C9(H9), C30(H30), C18(H18), C15(H15), C21(H21), C17(H17), C14(H14), C23(H23),
 C16(H16), C22(H22)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;