Synthesis and characterization of a luminescent and fully rigid tetrakisimidazolium macrocycle.
Zhou, Hongjun; Wang, Zhi; Gao, Chao; You, Jingsong; Gao, Ge; Chemical communications (Cambridge, England) 49 (2013) 1832–1834; doi:10.1039/c3cc38914f

data_7112307
_publ_section_title
;
 Synthesis and characterization of a luminescent and fully rigid
 tetrakisimidazolium macrocycle.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1832
_journal_page_last               1834
_journal_paper_doi               10.1039/c3cc38914f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         '2(Cl), C46 H52 N14 O6, 2(C H4 O), 3(H2 O)'
_chemical_formula_sum            'C48 H66 Cl2 N14 O11'
_chemical_formula_weight         1086.05
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-07
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.615(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9174(6)
_cell_length_b                   22.8283(7)
_cell_length_c                   16.9320(6)
_cell_measurement_reflns_used    5934
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      29.1164
_cell_measurement_theta_min      2.8697
_cell_volume                     5283.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130.0
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
1 omega -87.00 -37.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- -16.8924 -77.0000 60.0000 50
2 omega -9.00 34.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 19.8611 -95.0000 148.0000 43
3 omega -6.00 59.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 19.8611 77.0000 0.0000 65
4 omega -51.00 27.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 19.8611 -38.0000 -90.0000 78
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0263395000
_diffrn_orient_matrix_UB_12      -0.0265662000
_diffrn_orient_matrix_UB_13      -0.0051997000
_diffrn_orient_matrix_UB_21      -0.0240956000
_diffrn_orient_matrix_UB_22      0.0114435000
_diffrn_orient_matrix_UB_23      0.0252743000
_diffrn_orient_matrix_UB_31      -0.0377022000
_diffrn_orient_matrix_UB_32      0.0113021000
_diffrn_orient_matrix_UB_33      -0.0377399000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21229
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0023(5)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         9188
_refine_ls_number_restraints     828
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0743
_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^)+(0.0956P)^2^+7.6984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2037
_reflns_number_gt                6862
_reflns_number_total             9188
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108887
_cod_data_source_file            c3cc38914f.txt
_cod_data_source_block           ov_111201_s2_zhj
_cod_original_cell_volume        5283.2(3)
_cod_database_code               7112307
_chemical_oxdiff_formula         C20H20N2O2Cl2S1
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32