Modular Construction of a Porous Organometallic Network Based on Rhodium Olefin Complexation
Ulrich Stoeck; Georg Nickerl; Ulrich Burkhardt; Irena Senkovska; Stefan Kaskel; Journal of the American Chemical Society 134 (2012) 17335–17337; doi:10.1021/ja305482a

data_4118794
_publ_contact_author_address
;Department of Inorganic Chemistry
 Dresden University of Technology 
Bergstr. 66, 
01062 Dresden (Germany)
;
_publ_contact_author_email       stefan.kaskel@chemie.tu-dresden.de
_publ_contact_author_fax         (+49)351-4633-7287
_publ_contact_author_name        'Prof. Stefan Kaskel'
_publ_contact_author_phone       (+49)351-4633-4885
_publ_section_title
;
 Modular Construction of a Porous Organometallic Network Based on Rhodium
 Olefin Complexation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17335
_journal_page_last               17337
_journal_paper_doi               10.1021/ja305482a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C52 H44 Si'
_chemical_formula_sum            'C52 H44 Si'
_chemical_formula_weight         696.96
_chemical_name_common            tetra-(4-(7-norbonadienyl)-phenyl)-silan
_chemical_name_systematic        tetra-(4-(7-norbonadienyl)-phenyl)-silan
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      81
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.6000(17)
_cell_length_b                   16.6000(17)
_cell_length_c                   7.1395(7)
_cell_measurement_reflns_used    4396
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      1.23
_cell_volume                     1967.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 3.2e'
_computing_publication_material  encifer
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus 2007)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 180 frames, detector distance = 130 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13697
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.23
_diffrn_source
'sealed x-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       needles
_exptl_crystal_F_000             740
_exptl_crystal_recrystallization_method 'heptane, dichloromethane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0508P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                1793
_reflns_number_total             3719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305482a_si_001.cif
_cod_data_source_block           tetra-(4-(7-norbonadienyl)-phenyl)-silan
_cod_database_code               4118794