Anion complexation with cyanobenzoyl substituted first and second generation tripodal amide receptors: crystal structure and solution studies.
Hoque, Md Najbul; Gogoi, Abhijit; Das, Gopal; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15220–15231; doi:10.1039/c5dt00369e

data_7034933
_publ_section_title
;
 Anion complexation with cyanobenzoyl substituted first and second
 generation tripodal amide receptors: crystal structure and solution
 studies.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15220
_journal_page_last               15231
_journal_paper_doi               10.1039/c5dt00369e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H40 N7 O6, Cl O4'
_chemical_formula_sum            'C48 H40 Cl N7 O10'
_chemical_formula_weight         910.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.905(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.9320(10)
_cell_length_b                   18.5172(6)
_cell_length_c                   36.597(2)
_cell_measurement_reflns_used    15281
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.85
_cell_measurement_theta_min      2.18
_cell_volume                     10666.6(10)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.2176
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            55649
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3792.0
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         27403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.2866
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2438
_reflns_number_gt                15793
_reflns_number_total             27403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00369e2.cif
_cod_data_source_block           2LH-ClO4
_cod_depositor_comments
'Adding full bibliography for 7034925--7034934.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7034933
_plat606_alert_4_g
;
Problem: VERY LARGE Solvent Accessible VOID(S) in Structure        
Response: In this case there exists certain  amount  of  DMF-water  
solvent  trapped  in  the  crystal  lattice  in  a  disordered  
manner These electron densities were moved during refinement and 
the count of electron removed in total was 226 per two symmetry 
independent molecules which account for five DMF and three water molecules.
;