Easy Access to Silicon(0) and Silicon(II) Compounds
Kartik Chandra Mondal; Prinson P. Samuel; Mykyta Tretiakov; Amit Pratap Singh; Herbert W. Roesky; A. Claudia Stückl; Benedikt Niepötter; Elena Carl; Hilke Wolf; Regine Herbst-Irmer; Dietmar Stalke; Inorganic Chemistry 52 (2013) 4736–4743; doi:10.1021/ic400357p

data_4334543
_publ_contact_author_address
;University of G\"ottingen
Institut f\"ur Anorganische Chemie 
Tammannstra\&se 4
D-37077 G\"ottingen
Germany
;
_publ_contact_author_email       bniepoe@gwdg.de
_publ_contact_author_fax         '+49 551 393459''
_publ_contact_author_name        'Benedikt Niep\"otter'
_publ_contact_author_phone       '+49 551 393073'
_publ_section_title
;
 Easy Access to Silicon(0) and Silicon(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4736
_journal_page_last               4743
_journal_paper_doi               10.1021/ic400357p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C50 H71 N3'
_chemical_formula_sum            'C50 H71 N3'
_chemical_formula_weight         714.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 101.26(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1630(10)
_cell_length_b                   14.8070(10)
_cell_length_c                   21.0850(10)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.96
_cell_measurement_theta_min      3.4695
_cell_volume                     4336.7(6)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'shelXle v0.477'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48500
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.284
_diffrn_reflns_theta_min         3.469
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/4
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8161
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0553P)^2^+1.4810P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7785
_reflns_number_total             8161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400357p_si_001_4.cif
_cod_data_source_block           5
_cod_database_code               4334543
_shelxl_version_number           2012-6
_shelx_res_checksum              61067