Crystal structure of 1,1'-methylenedipyridinium dibromide monohydrate, (C11H12N2)Br2 • H2O
Zhi-Fang Zhang; Zeitschrift für Kristallographie - New Crystal Structures 226 (2011) 553–; doi:

data_8103223
_publ_contact_author
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     Z.F. Zhang
School of Chemistry and Chemical Engineering, Yulin University,
      Yulin 719000, P. R. China
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_publ_section_title
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 Crystal structure of 1,1'-methylenedipyridinium dibromide monohydrate,
 (C11H12N2)Br2 &#x2022; H2O
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              553
_journal_volume                  226
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H12 N2, H2 O, 2(Br)'
_chemical_formula_sum            'C11 H14 Br2 N2 O'
_chemical_formula_weight         350.06
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
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2011-03-20 # Formatted by publCIF
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.364(3)
_cell_length_b                   16.814(2)
_cell_length_c                   8.1486(9)
_cell_measurement_reflns_used    7942
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.97
_cell_volume                     2653.1(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega 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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10484
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    6.093
_exptl_absorpt_correction_T_max  0.219
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details 'Flack (1983), 451 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.004(18)
_refine_ls_extinction_coef       0.0075(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1281
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0401P)^2^+0.6115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                1177
_reflns_number_total             1281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3548.cff
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z 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 
;
_cod_original_sg_symbol_Hall     F2-2d
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               8103223
_publ_section_exptl_
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All H atoms on C were placed in idealized 
positions and refined as riding atoms with on their parent atoms with
C--H distances of 0.93\%A,  U~iso~(H)= 1.2 U~eq~(C), d(O-H)= 0.85\%A
U~iso~(H)=1.5 U~eq~(O).One of the hydrogen atom (H1B) attached to the 
oxygen atom (O(1) of the water molecue was located at general position
 with S.O.F of 0.5, e.g. halfly-occupied.
;