A Pyrrolyl-Based Triazolophane: A Macrocyclic Receptor With CH and NH Donor Groups That Exhibits a Preference for Pyrophosphate Anions
Jonathan L. Sessler; Jiajia Cai; Han-Yuan Gong; Xiaoping Yang; Jonathan F. Arambula; Benjamin P. Hay; Journal of the American Chemical Society 132 (2010) 14058–14060; doi:10.1021/ja107098r

data_4103243
_publ_section_title
;
 A Pyrrolyl-Based Triazolophane: A Macrocyclic Receptor With CH and NH
 Donor Groups That Exhibits a Preference for Pyrophosphate Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14058
_journal_page_last               14060
_journal_paper_doi               10.1021/ja107098r
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C50 H52 N16, 3(C16 H36 N), O7 P2, 3(O)'
_chemical_formula_sum            'C98 H160 N19 O10 P2'
_chemical_formula_weight         1826.39
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.507(4)
_cell_length_b                   39.237(8)
_cell_length_c                   24.684(5)
_cell_measurement_reflns_used    33540
_cell_measurement_temperature    113(1)
_cell_measurement_theta_max      31.1049
_cell_measurement_theta_min      1.2180
_cell_volume                     12695(8)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      113(1)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            89512
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'DENZO and Scalepack (Otwinoski and Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3964
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00045(18)
_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   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         21480
_refine_ls_number_restraints     779
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0979
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1842P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2669
_refine_ls_wR_factor_ref         0.2973
_reflns_number_gt                12530
_reflns_number_total             21480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107098r_si_002.cif
_cod_data_source_block           complex-1
_cod_original_cell_volume        12694(4)
_cod_database_code               4103243