Donor-extended tripodal pyrroles: encapsulation, metallation, and H-bonded tautomers
John S. Hart; Fraser J. White; Jason B. Love; Chem.Commun. 47 (2011) 5711–; doi:10.1039/c1cc11378j

data_7106410
_publ_section_title
;
 Donor-extended tripodal pyrroles: encapsulation, metallation, and
 H-bonded tautomers
;
_journal_name_full               Chem.Commun.
_journal_page_first              5711
_journal_paper_doi               10.1039/c1cc11378j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C100 H156 Li12 N12 O13.5'
_chemical_formula_weight         1825.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-03-08T12:25:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.511(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2257(5)
_cell_length_b                   20.6980(6)
_cell_length_c                   20.3016(6)
_cell_measurement_reflns_used    8223
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0853
_cell_measurement_theta_min      2.8916
_cell_volume                     5634.4(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37811
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.9
_diffrn_standards_number         38440
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.93142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         13199
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.254
_reflns_number_gt                5744
_reflns_number_total             13199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11378j.txt
_cod_data_source_block           j10015
_cod_original_formula_sum        'C100 H156 Li12 N12 O13.50'
_cod_database_code               7106410