Synthesis and Structural Characterization of Base-Stabilized Oligomeric Heterovinylidenes
Wing-Por Leung; Wang-Kin Chiu; Thomas C. W. Mak; Inorganic Chemistry 52 (2013) 9479–9486; doi:10.1021/ic4011345

data_4335751
_publ_section_title
;
 Synthesis and Structural Characterization of Base-Stabilized Oligomeric
 Heterovinylidenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9479
_journal_page_last               9486
_journal_paper_doi               10.1021/ic4011345
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C36 H46 Li N O2 P2 Si'
_chemical_formula_weight         621.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.857(4)
_cell_angle_beta                 100.286(3)
_cell_angle_gamma                96.741(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7296(19)
_cell_length_b                   10.880(2)
_cell_length_c                   16.270(3)
_cell_measurement_reflns_used    1015
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.53
_cell_volume                     1841.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0585
_diffrn_reflns_av_sigmaI/netI    0.1424
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10061
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.106125
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.2043
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.3062
_reflns_number_gt                2397
_reflns_number_total             6450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4011345_si_003.cif
_cod_data_source_block           cwk6
_cod_database_code               4335751