[Bis(<i>o</i>-dimethylaminomethylphenyl)methylsilanol-<i>N</i>,<i>O</i>]dibromocobalt(II)
Baggio, R. F.; Garland, M. T.; Manzur, J.; Spodine, E.; Acta Crystallographica Section C 51 (1995) 602–604; doi:10.1107/S0108270194009200

data_2003312
_publ_section_title
'[Bis(<i>o</i>-dimethylaminomethylphenyl)methylsilanol-<i>N</i>,<i>O</i>]dibromocobalt(II)'
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              602
_journal_page_last               604
_journal_paper_doi               10.1107/S0108270194009200
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;Tris(o-N,N-dimethylaminomethylphenyl)methylsilane was prepared by the
reaction of (\o-N,N-dimethylaminomethyl)phenyl lithium with
methyltrichlorosilane, 1:1 molar ratio, in ether--tetrahydrofuran. The
reacting mixture was stirred for 24 h, filtered, and the solution was
evaporated until an oily residue was obtained. This residue was dissolved
in acetonitrile and a crystalline product was obtained from this solution.
The ligand was characterized by ^1^H NMR spectroscopy using a CCl~4~
solution with an internal standard of tetramethylsilane (TMS). Characteristic
peaks were obtained at 7.0-7.6 (multiplet, corresponding
to 12H of the phenyl rings),
3.25 (singlet, corresponding to 6H of methylene groups
bonded to
the phenyl rings), 2.0 (singlet, corresponding to 18H of methyl groups
bonded to N atoms) and 0.93 p.p.m. (singlet, corresponding to 3H of methyl
group bonded to the Si atom). Anhydrous CoBr~2~ was added to a freshly
prepared solution of the ligand in acetonitrile. This solution gave blue
crystals of the title complex on standing.
;
_chemical_formula_moiety         'Co Br~2~ (C19 H28 N2 O Si)'
_chemical_formula_sum            'C19 H28 Br2 Co N2 O Si'
_chemical_formula_weight         547.3
_chemical_name_common
;
?
;
_chemical_name_systematic
;
Dibromo[bis(o-N,N-dimethylaminomethylphenyl)methylsilanol]cobalt(II)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   11.8440(10)
_cell_length_b                   12.8710(10)
_cell_length_c                   15.237(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     2322.8(4)
_computing_cell_refinement       P3/P4-PC
_computing_data_collection       'P3/P4-PC (Siemens, 1991)'
_computing_data_reduction        'XDISK in SHELXTL/PC (Sheldrick, 1991)'
_computing_molecular_graphics    'XP in SHELXTL/PC'
_computing_publication_material  'XPUBL in SHELXTL/PC'
_computing_structure_refinement  'XLS in SHELXTL/PC'
_computing_structure_solution    'XS in SHELXTL/PC'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Siemens R3m difractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            2329
_diffrn_reflns_reduction_process 2231
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   'Semi-mpirical (\y scans)'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.83
_refine_ls_hydrogen_treatment
'Idealized H-atom positions riding on host atom'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     235
_refine_ls_number_reflns         1784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_obs          0.039
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F) + 0.0021F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.055
_refine_ls_wR_factor_obs         0.049
_reflns_number_observed          1784
_reflns_number_total             2231
_reflns_observed_criterion       4.0
_cod_data_source_file            bk1030.cif
_cod_data_source_block           LbaCo
_cod_depositor_comments
;
 Removing the "\" symbol from the _chemical_name_systematic
 data item value.

 Antanas Vaitkus,
 2017-03-29

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F) + 0.0021F^2^]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(F) +
0.0021F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2322.7(5)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2003312