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_7200670
_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_absolute_configuration ad
_chemical_formula_moiety         'C35 H27 Br2 N3 O3, C H Cl3'
_chemical_formula_sum            'C36 H28 Br2 Cl3 N3 O3'
_chemical_formula_weight         816.80
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.8561(4)
_cell_length_b                   53.1999(16)
_cell_length_c                   15.4900(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    223
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     13890.5(7)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       74
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24246
_diffrn_reflns_theta_full        30.038
_diffrn_reflns_theta_max         30.038
_diffrn_reflns_theta_min         1.531
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.606
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.022(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0671
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.002640
_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:
0.213 -0.941 -0.124 -0.456
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0308
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0267
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              74
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                7744
_reflns_number_total             9756
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0300
_oxford_refine_ls_scale          0.09364(6)
_oxford_reflns_number_all        9725
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b819927b.txt
_cod_data_source_block           1
_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 
;
_cod_original_sg_symbol_Hall     'F 2 -2d '
_cod_original_sg_symbol_H-M      'F d d 2 '
_cod_database_code               7200670