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_7034930
_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         '4(C48 H40 N7 O6), 4(F2 H), 2(H2 O), H4 O '
_chemical_formula_sum            'C192 H172 F8 N28 O27'
_chemical_formula_weight         3455.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-04-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.02.26 svn.r3159 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-04-23 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.627(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.7467(16)
_cell_length_b                   18.6826(16)
_cell_length_c                   16.7739(11)
_cell_measurement_reflns_used    12652
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.5367
_cell_measurement_theta_min      1.5852
_cell_volume                     8374.5(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_laue_measured_fraction_full 0.982
_diffrn_reflns_laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28319
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.370
_diffrn_reflns_theta_max         24.370
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       needle
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.991
_exptl_transmission_factor_min   0.982
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1233P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4867
_reflns_number_total             6757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00369e2.cif
_cod_data_source_block           4LH-4HF2-3H2O
_cod_depositor_comments
'Adding full bibliography for 7034925--7034934.cif.'
_cod_database_code               7034930
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O7-H7B_$1
 0.85 with sigma of 0.02
 O7A-H7AA
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O7A(0.25)
4.a Riding coordinates:
 F2(H1C)
4.b Ternary CH refined with riding coordinates:
 N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C17(H17A,H17B), C18(H18A,H18B), C34(H34A,H34B),
 C33(H33A,H33B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C5(H5), C7(H7), C4(H4A), C8(H8), C14(H14), C11(H11), C15(H15),
  C16(H16), C24(H24), C23(H23), C20(H20), C21(H21), C26(H26), C29(H29),
 C30(H30), C32(H32), C37(H37), C39(H39), C36(H36), C40(H40), C41(H41), C46(H46),
  C42(H42), C44(H44), N7(H7A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'