Synthesis and X-ray Structures of Novel Macrocycles and Macrobicycles Containing N,N-Di(pyrrolylmethyl)-N-methylamine Moiety: Preliminary Anion Binding Study
Rajnish Kumar; Tapas Guchhait; Ganesan Mani; Inorganic Chemistry 51 (2012) 9029–9038; doi:10.1021/ic3011822

data_4330087
_publ_contact_author_address
;Department of Chemistry
Indian Institute of Technology-Kharagpur
Kharagpur, India 721 302
;
_publ_contact_author_email       gmani@chem.iitkgp.ernet.in
_publ_contact_author_fax         91-3222-282252
_publ_contact_author_name        'Mani, Ganesan.'
_publ_contact_author_phone       91-3222-282320
_publ_section_title
;
 Synthesis and X-ray Structures of Novel Macrocycles and Macrobicycles
 Containing N,N-Di(pyrrolylmethyl)-N-methylamine Moiety: Preliminary Anion
 Binding Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9029
_journal_page_last               9038
_journal_paper_doi               10.1021/ic3011822
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C51 H80.32 N17 O5.16'
_chemical_formula_weight         1014.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.956(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.044(3)
_cell_length_b                   11.7179(12)
_cell_length_c                   34.807(5)
_cell_measurement_reflns_used    70341
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.87
_cell_volume                     12265(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            70341
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4373
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 2172 A^3^ and 312 e, respectively. For Z = 8 this gives
39 electrons per formula. This number equals 2.16 molecules of solvent water. 
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10736
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1818P)^2^+0.4668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2746
_reflns_number_gt                6887
_reflns_number_total             10736
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3011822_si_002_5.cif
_cod_data_source_block           bicycle-7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4330087