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_7034931
_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, Br'
_chemical_formula_sum            'C48 H40 Br N7 O6'
_chemical_formula_weight         890.77
_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
_audit_update_record
;
2015-04-10 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                91.493(3)
_cell_angle_beta                 94.733(2)
_cell_angle_gamma                103.295(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4588(5)
_cell_length_b                   13.6915(7)
_cell_length_c                   20.4866(10)
_cell_measurement_reflns_used    12652
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      1.91
_cell_volume                     2570.4(2)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39258
_diffrn_reflns_theta_full        28.65
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             920.0
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         13168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1852
_reflns_number_gt                7346
_reflns_number_total             13138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00369e2.cif
_cod_data_source_block           2LH-Br
_cod_depositor_comments
'Adding full bibliography for 7034925--7034934.cif.'
_cod_database_code               7034931
_plat606_alert_4_g
;
Problem:VERY LARGE Solvent Accessible VOID(S) in Structure
Response: SQUEEZE has been performed to the disordered solvent molecule. 
This calculated amount of 554 electrons per unit cell or 98 electrons per 
molecule may be attributed to two water and two DMF molecules.
;