Syntheses of Group 7 Metal Carbonyl Complexes with a Stable N-Heterocyclic Chlorosilylene
Ramachandran Azhakar; Sankaranarayana Pillai Sarish; Herbert W. Roesky; Jakob Hey; Dietmar Stalke; Inorganic Chemistry 50 (2011) 5039–5043; doi:10.1021/ic2003035

data_4325212
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_contact_author_email       dstalke@chemie.uni-goettingen.de
_publ_section_title
;
 Syntheses of Group 7 Metal Carbonyl Complexes with a Stable
 N-Heterocyclic Chlorosilylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5039
_journal_page_last               5043
_journal_paper_doi               10.1021/ic2003035
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C48 H69 Cl3 N6 O3 Re Si3, C7 H8, C5 O5 Re'
_chemical_formula_sum            'C60 H77 Cl3 N6 O8 Re2 Si3'
_chemical_formula_weight         1573.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.4560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4470(4)
_cell_length_b                   37.8010(13)
_cell_length_c                   14.4401(5)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.623
_cell_measurement_theta_min      2.155
_cell_volume                     6794.0(4)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v.2010.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XP in SHELXTL Version 2008/3'
_computing_publication_material  'XP in SHELXTL Version 2008/3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II with D8 goniometer'
_diffrn_measurement_method       'omega scans and phi scans'
_diffrn_radiation_monochromator  'INCOATEC mirror optics'
_diffrn_radiation_source         'INCOATEC I\mS Mo Microfocus Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            272786
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    3.785
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       needle
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.867
_refine_diff_density_min         -1.939
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         14417
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+54.0202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                13147
_reflns_number_total             14417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003035_si_002.cif
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4325212