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_7039588
_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_formula_sum            'C34 H56 F6 N6 O2 Si'
_chemical_formula_weight         722.93
_chemical_name_systematic
;
 ?
;
_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_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                 99.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.93(2)
_cell_length_b                   10.616(16)
_cell_length_c                   27.70(4)
_cell_measurement_reflns_used    13255
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.995
_cell_measurement_theta_min      1.489
_cell_volume                     3753(10)
_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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1183
_diffrn_reflns_av_unetI/netI     0.1671
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14408
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.345
_diffrn_reflns_theta_min         1.489
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.049
_platon_squeeze_details
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 648\%A^3^ and 168 e, respectively. These numbers suggest 
roughly 2 molecules of solvent methanol per formula or 8 molecules 
per unit cell. 
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3904
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1619
_reflns_number_total             3904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01396a2.cif
_cod_data_source_block           2h
_cod_depositor_comments
'Adding full bibliography for 7039581--7039589.cif.'
_cod_database_code               7039588
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-3
_shelx_res_checksum              59905