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_7200671
_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         'C37 H27 N5 O3'
_chemical_formula_sum            'C37 H27 N5 O3'
_chemical_formula_weight         589.65
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-05-29
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                71.544(2)
_cell_angle_beta                 88.809(2)
_cell_angle_gamma                80.093(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8089(4)
_cell_length_b                   11.1946(4)
_cell_length_c                   14.5862(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    223
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1495.66(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.028
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53005
_diffrn_reflns_theta_full        29.508
_diffrn_reflns_theta_max         30.111
_diffrn_reflns_theta_min         2.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.000386
_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:
0.601 0.537 0.267
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0690
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0495
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5817
_reflns_number_total             8757
_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          0.6335(9)
_oxford_structure_analysis_title 'gq1_223k_0m in P-1'
_cod_data_source_file            b819927b.txt
_cod_data_source_block           gq1_223k
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 -1 '
_cod_database_code               7200671