Synthesis, Solid-State Structures, and Computational Studies of Half-Sandwich Cp*BeX (X = Cl, Br, I) Compounds
Naglav, Dominik; Tobey, Briac; Neumann, Anja; Bläser, Dieter; Wölper, Christoph; Schulz, Stephan; Organometallics 34 (2015) 3072–; doi:10.1021/acs.organomet.5b00389

data_4087602
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universit\"at Duisburg-Essen
         Campus Essen, Universit\"atsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Synthesis, Solid-State Structures, and Computational Studies of
 Half-Sandwich Cp*BeX (X = Cl, Br, I) Compounds
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3072
_journal_paper_doi               10.1021/acs.organomet.5b00389
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C10 H15 Be Br'
_chemical_formula_weight         224.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                79.197(2)
_cell_angle_beta                 73.809(2)
_cell_angle_gamma                73.991(2)
_cell_formula_units_Z            4
_cell_length_a                   7.9899(3)
_cell_length_b                   11.5328(5)
_cell_length_c                   12.3940(5)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.75
_cell_measurement_theta_min      2.73
_cell_volume                     1046.64(7)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24232
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.280
_diffrn_reflns_theta_min         1.723
_exptl_absorpt_coefficient_mu    3.871
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       tablet
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5853
_reflns_number_total             7688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00389_si_002.cif
_cod_data_source_block           dnp_075m
_cod_original_cell_volume        1046.64(8)
_cod_database_code               4087602
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.378
_shelx_estimated_absorpt_t_max   0.712
_shelx_res_checksum              45649
_shelx_hkl_checksum              23749