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_4335749
_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            'C84 H87 Ge3 N3 P6 Si3'
_chemical_formula_weight         1626.43
_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                86.2080(10)
_cell_angle_beta                 78.4490(10)
_cell_angle_gamma                89.7510(10)
_cell_formula_units_Z            4
_cell_length_a                   16.6973(8)
_cell_length_b                   22.7980(11)
_cell_length_c                   23.5002(12)
_cell_measurement_reflns_used    244
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     8745.0(7)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_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  0.1179
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97744
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.6972
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         1.895
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         31621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                17877
_reflns_number_total             31621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4011345_si_001.cif
_cod_data_source_block           OC120
_cod_database_code               4335749