Synthesis and structural characterization of anion complexes with azacalix[2]dipyrrolylmethane: effect of anion charge on the conformation of the macrocycle.
Guchhait, Tapas; Mani, Ganesan; Schulzke, Carola; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11781–11790; doi:10.1039/c6dt01396a

data_7039589
_publ_section_title
;
 Synthesis and structural characterization of anion complexes with
 azacalix[2]dipyrrolylmethane: effect of anion charge on the conformation
 of the macrocycle.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11781
_journal_page_last               11790
_journal_paper_doi               10.1039/c6dt01396a
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_sum            'C32 H48 N6 O3 S2'
_chemical_formula_weight         628.88
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-06-13 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.19(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.660(9)
_cell_length_b                   11.998(9)
_cell_length_c                   11.826(9)
_cell_measurement_reflns_used    23895
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.511
_cell_volume                     1653(2)
_computing_data_collection       APEX2
_computing_molecular_graphics    Diamond3.2
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.823
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1222
_diffrn_reflns_av_unetI/netI     0.1787
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
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_diffrn_reflns_number            12097
_diffrn_reflns_point_group_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.999
_diffrn_reflns_theta_min         3.740
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       Prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.060
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_refine_diff_density_max         0.224
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 720 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_coef       0.0080(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.711
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                2310
_reflns_number_total             4602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01396a2.cif
_cod_data_source_block           2i
_cod_depositor_comments
'Adding full bibliography for 7039581--7039589.cif.'
_cod_database_code               7039589
_shelx_estimated_absorpt_t_min   0.616
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-3
_shelx_res_checksum              25098