Bromo(hydrido)methylbis(4-methylpyridine-<i>N</i>)silicon Bromide at 173K
Hensen, Karl; Kettner, Markus; Bolte, Michael; Acta Crystallographica Section C 54 (1998) 358–359; doi:10.1107/S0108270197015801

data_2007099
_publ_section_title
;
 Bromo(hydrido)methylbis(4-methylpyridine-<i>N</i>)silicon Bromide at
 173K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              358
_journal_page_last               359
_journal_paper_doi               10.1107/S0108270197015801
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C13 H18 Br N2 Si 1+, Br 1-'
_chemical_formula_sum            'C13 H18 Br2 N2 Si'
_chemical_formula_weight         390.20
_chemical_name_systematic
;
Bromohydridomethyl-bis-(4-Methylpyridinium)-siliciumbromid
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.39720(10)
_cell_length_b                   12.39170(10)
_cell_length_c                   13.7857(2)
_cell_measurement_reflns_used    5772
_cell_measurement_temperature    173
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     1605.31(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL96 (Sheldrick, 1996b)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Siemens CCD three-circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17926
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  840
_diffrn_standards_number         305
_exptl_absorpt_coefficient_mu    5.111
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   'Empirical using SADABS (Sheldrick, 1996a)'
_exptl_crystal_colour            'colourless, transparent'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.399
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.033
_refine_ls_R_factor_obs          .024
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0135P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.043
_refine_ls_wR_factor_obs         .042
_reflns_number_observed          2576
_reflns_number_total             2950
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1258.cif
_cod_data_source_block           he2sad
_cod_depositor_comments
;
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_enum 1527 2010-12-29 10:47:43Z saulius 

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 'calc w =
1/[\s^2^(Fo^2^)+(0.0135P)^2^] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0135P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2007099
_cod_database_fobs_code          2007099