Reactions of an Iron Chlorodistannane with Hydroxide: Isolation and Structural Characterization of {(η5-Me3SiC5H4)Fe(CO)[(SntBu2)2(μ-OH)]···DMAP}, DMAP = 4-(N,N-Dimethylamino)pyridine, a μ-OH-Stannyl(stannylene)‒Iron Complex
Sharma, Hemant K.; Metta-Magaña, Alejandro J.; Pannell, Keith H.; Organometallics 32 (2013) 6218–; doi:10.1021/om3012129

data_4089397
_publ_section_title
;
 Reactions of an Iron Chlorodistannane with Hydroxide: Isolation and
 Structural Characterization of
 {(\h5-Me3SiC5H4)Fe(CO)[(SntBu2)2(\m-OH)]&#x00B7;&#x00B7;&#x00B7;DMAP},
 DMAP = 4-(N,N-Dimethylamino)pyridine, a \m-OH-Stannyl(stannylene)--Iron
 Complex
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6218
_journal_paper_doi               10.1021/om3012129
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C25 H56 Fe O2 Si Sn2, C7 H4 N2'
_chemical_formula_sum            'C32 H60 Fe N2 O2 Si Sn2'
_chemical_formula_weight         826.14
_chemical_name_systematic
; 
 (\u^2-Hydroxo)-(carbonyl)-(trimethylsilyl-
 \n^5-cyclopentadienyl)-tetrakis(t-butyl)-
 iron-di-tin(ii)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.114(2)
_cell_angle_beta                 100.116(2)
_cell_angle_gamma                114.472(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8120(11)
_cell_length_b                   11.7799(17)
_cell_length_c                   18.284(2)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.498
_cell_measurement_theta_min      2.297
_cell_volume                     1874.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6528
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  0.7980
_exptl_absorpt_correction_T_min  0.7193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6528
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.247
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0185
_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^)+(0.1000P)^2^+0.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6074
_reflns_number_total             6528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            11.cif
_cod_data_source_block           twin4sa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1874.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089397