Large shape-persistent metal-invertible 15-Nsp2-donor-atom macrocycles functioning as trinucleating ligands
Adrian-Mihail Stadler; Ji-Jun Jiang; Hai-Ping Wang; Corinne Bailly; Chem.Commun. 49 (2013) 3784–; doi:10.1039/c2cc37260f

data_7109149
_publ_section_title
;
 Large shape-persistent metal-invertible 15-Nsp2-donor-atom macrocycles
 functioning as trinucleating ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              3784
_journal_paper_doi               10.1039/c2cc37260f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C35 H34 F9 N14 O10 Pb2 S3, C F3 O3 S, C H3 N O2'
_chemical_formula_sum            'C37 H37 F12 N15 O15 Pb2 S4'
_chemical_formula_weight         1702.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                69.747(1)
_cell_angle_beta                 68.929(1)
_cell_angle_gamma                77.743(1)
_cell_formula_units_Z            2
_cell_length_a                   12.0938(7)
_cell_length_b                   15.8194(9)
_cell_length_c                   16.3813(10)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.39
_cell_volume                     2729.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44044
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    6.431
_exptl_absorpt_correction_T_max  0.5656
_exptl_absorpt_correction_T_min  0.3595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.147
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         15903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+19.8958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                10437
_reflns_number_total             15903
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc37260f.txt
_cod_data_source_block           jmlms120821
_cod_database_code               7109149