Phase-separated hydrogen-bonded chloride ion–water–oxonium ion sheets and protonated 4′-(4-bromophenyl)-2,2′:6′,2″-terpyridine stacks, and condensation products of 2-acetylpyridine and benzaldehydes revisited
Constable, Edwin C.; Zhang, Guoqi; Housecroft, Catherine E.; Neuburger, Markus; Schaffner, Silvia; CrystEngComm 11 (2009) 1014–; doi:10.1039/b819927b

data_7200669
_publ_section_title
;
 Phase-separated hydrogen-bonded chloride ion--water--oxonium ion
 sheets and protonated
 4&#x2032;-(4-bromophenyl)-2,2&#x2032;:6&#x2032;,2&#x2033;-terpyridine
 stacks, and condensation products of 2-acetylpyridine and
 benzaldehydes revisited
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1014
_journal_paper_doi               10.1039/b819927b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C21 H16 Br N3, H3 O, 3(H2 O), 3(Cl)'
_chemical_formula_sum            'C21 H25 Br Cl3 N3 O4'
_chemical_formula_weight         569.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-10-13
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 93.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3916(2)
_cell_length_b                   28.4550(10)
_cell_length_c                   12.1415(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    223
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2547.77(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31822
_diffrn_reflns_theta_full        29.268
_diffrn_reflns_theta_max         29.865
_diffrn_reflns_theta_min         1.827
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.959
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0614
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3870
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001463
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.540 0.562 0.340 0.731E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0636
_refine_ls_wR_factor_gt          0.0311
_refine_ls_wR_factor_ref         0.0311
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3870
_reflns_number_total             7235
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1941(2)
_oxford_structure_analysis_title 'gq4_223k_0m in P2(1)/n'
_cod_data_source_file            b819927b.txt
_cod_data_source_block           gq4_223k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C21 H25 Br1 Cl3 N3 O4'
_cod_database_code               7200669