Hydrated anion glued capsular and non-capsular assembly of a tripodal host: Solid state recognition of bromide‒water [Br5‒(H2O)6]5− and iodide‒water [I2‒(H2O)4]2− clusters in cationic tripodal receptor
Hoque, Md. Najbul; Das, Gopal; CrystEngComm 16 (2014) 4447–; doi:10.1039/c4ce00149d

data_7214377
_publ_section_title
;
 Hydrated anion glued capsular and non-capsular assembly of a tripodal
 host: Solid state recognition of bromide--water [Br5--(H2O)6]5&#x2212;
 and iodide--water [I2--(H2O)4]2&#x2212; clusters in cationic tripodal
 receptor
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              4447
_journal_paper_doi               10.1039/c4ce00149d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C24 H34 N4 O3, 4(I), 7/4(H2 O)'
_chemical_formula_sum            'C24 H37.5 I4 N4 O4.75'
_chemical_formula_weight         965.67
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.377(2)
_cell_angle_beta                 87.245(2)
_cell_angle_gamma                88.453(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6814(6)
_cell_length_b                   13.0383(6)
_cell_length_c                   20.9938(10)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.56
_cell_volume                     3354.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42264
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    3.750
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1832.00
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.107
_refine_diff_density_min         -3.423
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         14556
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+19.7972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                8849
_reflns_number_total             15796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00149d2.cif
_cod_data_source_block           '[4LH4-16I-7H2O]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7214372--7214377.cif.

2018-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H150 I16 N16 O19'
_cod_original_formula_weight         3862.67
_cod_original_formula_moiety         '4(C24 H34 N4 O3), O2, 16(I), 4(H2 O), O'
_cod_original_formula_units_Z            1
_cod_database_code               7214377