Preparation and Photophysical Properties of Phosphino- and Phosphine Oxide-Linked Siloles
Braddock-Wilking, Janet; Gao, Li-Bin; Rath, Nigam P.; Organometallics 29 (2010) 1612–; doi:10.1021/om900956u

data_4067434
_publ_section_title
;
 Preparation and Photophysical Properties of Phosphino- and Phosphine
 Oxide-Linked Siloles
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1612
_journal_paper_doi               10.1021/om900956u
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C54 H44 O2 P2 Si'
_chemical_formula_weight         814.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.087(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.5999(13)
_cell_length_b                   16.7822(19)
_cell_length_c                   44.176(5)
_cell_measurement_reflns_used    4990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      2.80
_cell_volume                     8534.1(17)
_computing_cell_refinement       'Bruker-Apex II (Bruker, 2006)'
_computing_data_collection       'Bruker-Apex II (Bruker, 2006)'
_computing_data_reduction        'Bruker-SAINT   (Bruker, 2006)'
_computing_molecular_graphics
'Bruker-SHELXTL (Sheldrick, G.M. (2008). Acta Cryst. A64,112-122)'
_computing_publication_material
'Bruker-SHELXTL (Sheldrick, G.M. (2008). Acta Cryst. A64,112-122)'
_computing_structure_refinement
'Bruker-SHELXTL (Sheldrick, G.M. (2008). Acta Cryst. A64,112-122)'
_computing_structure_solution
'Bruker-SHELXTL (Sheldrick, G.M. (2008). Acta Cryst. A64,112-122)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.2012
_diffrn_reflns_av_sigmaI/netI    0.1390
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            166532
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.8703
_exptl_absorpt_correction_T_min  0.8119
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'sadabs v2007/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         14998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+3.8529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2409
_reflns_number_gt                7391
_reflns_number_total             14998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900956u_si_003.cif
_cod_data_source_block           w19907
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8534.2(16)
_cod_original_sg_symbol_H-M      P2~1~/n
_cod_database_code               4067434