1,2-Halosilane vs. 1,2-alkylborane elimination from (boryl)(silyl) complexes of iron: switching between borylenes and silylenes just by changing the alkyl group
Holger Braunschweig; Rian D. Dewhurst; Krzysztof Radacki; Benedikt Wennemann; Qing Ye; Chem.Commun. 51 (2015) 15465–; doi:10.1039/C5cc06425B

data_7117928
_publ_section_title
;
 1,2-Halosilane vs. 1,2-alkylborane elimination from (boryl)(silyl)
 complexes of iron: switching between borylenes and silylenes just by
 changing the alkyl group
;
_journal_name_full               Chem.Commun.
_journal_page_first              15465
_journal_paper_doi               10.1039/C5cc06425B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C19 H38 Fe2 O5 P2 Si2'
_chemical_formula_sum            'C19 H38 Fe2 O5 P2 Si2'
_chemical_formula_weight         576.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   other
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-27 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1382(6)
_cell_length_b                   12.4474(8)
_cell_length_c                   11.8729(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.24
_cell_volume                     1340.86(15)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'Smart NT ver. 5.63 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector (Apex1)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART-APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.874
_diffrn_reflns_theta_min         1.728
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/4 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5701
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.904
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.983
_reflns_number_gt                5521
_reflns_number_total             5701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc06425b2.cif
_cod_data_source_block           7c
_cod_database_code               7117928
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              66757