Cocrystallization of pyrogallol[4]arenes with 1-(2-pyridylazo)-2-naphthol
Pfeiffer, Constance R.; Fowler, Drew A.; Teat, Simon; Atwood, Jerry L.; CrystEngComm 16 (2014) 10760–; doi:10.1039/C4CE01768D

data_7218222
_publ_section_title
;
 Cocrystallization of pyrogallol[4]arenes with 1-(2-pyridylazo)-2-naphthol
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              10760
_journal_paper_doi               10.1039/C4CE01768D
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C40 H48 O16, C15 H11 O1 N3, C2 H6 O1'
_chemical_formula_sum            'C57 H65 N3 O18'
_chemical_formula_weight         1080.12
_chemical_name_common
'C-propylpyrogallol[4]arene with 1-(2-pyridylazo)-2-napthol'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                84.294(2)
_cell_angle_beta                 85.839(2)
_cell_angle_gamma                63.720(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8485(16)
_cell_length_b                   12.7498(17)
_cell_length_c                   18.287(2)
_cell_measurement_reflns_used    5271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2
_cell_measurement_theta_min      3.2
_cell_volume                     2463.5(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-1997 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-1997 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33711
_diffrn_reflns_theta_full        32.07
_diffrn_reflns_theta_max         32.07
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Advanced Light Source Station 11.3.1'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         13132
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+1.0413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1850
_reflns_number_gt                9453
_reflns_number_total             13132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01768d1.cif
_cod_data_source_block           2cp81h
_cod_depositor_comments
'Adding full bibliography for 7218212--7218223.cif.'
_cod_database_code               7218222