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_4089395
_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_sum            'C36 H61 Cl Fe2 O4 Si2 Sn2'
_chemical_formula_weight         998.56
_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                78.988(2)
_cell_angle_beta                 73.602(2)
_cell_angle_gamma                67.163(2)
_cell_formula_units_Z            2
_cell_length_a                   12.873(2)
_cell_length_b                   12.877(2)
_cell_length_c                   15.636(3)
_cell_measurement_reflns_used    5158
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.29
_cell_volume                     2281.8(7)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33024
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_correction_T_min  0.7417
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.784
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         10966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.002
_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^+0.5962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                6961
_reflns_number_total             10966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            7.cif
_cod_data_source_block           529hs_0ms
_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        2282.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089395