Synthesis of Alkynyl-Substituted 9,10-Dimetallatriptycenes of Group 14 and Their Application in the Preparation of a Novel Class of Organometallic Oligomers
Dam, Matheus A.; Hoogervorst, Wilhelmus J.; de Kanter, Franciscus J. J.; Bickelhaupt, Friedrich; Spek, Anthony L.; Organometallics 17 (1998) 1762–; doi:10.1021/om980073f

data_4078399
_publ_section_title
;
 Synthesis of Alkynyl-Substituted 9,10-Dimetallatriptycenes of Group 14
 and Their Application in the Preparation of a Novel Class of
 Organometallic Oligomers
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1762
_journal_paper_doi               10.1021/om980073f
_journal_volume                  17
_journal_year                    1998
_chemical_formula_sum            'C55 H36.5 Cl0.5 Ge4'
_chemical_formula_weight         1005.56
_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                72.697(12)
_cell_angle_beta                 80.666(11)
_cell_angle_gamma                79.253(11)
_cell_formula_units_Z            2
_cell_length_a                   8.4807(11)
_cell_length_b                   12.9985(19)
_cell_length_c                   21.141(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2171.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CAD4-T
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10624
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    2.841
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+2.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                7480
_reflns_number_total             9945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om980073f.cif
_cod_data_source_block           s1665b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+2.5065P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+2.5065P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C52H34Ge4, 0.5(C6H5Cl)'
_cod_database_code               4078399