Stacking Interactions Drive Selective Self-Assembly and Self-Sorting of Pyrene-Based M(II)4L6 Architectures.
Ronson, Tanya K.; Roberts, Derrick A.; Black, Samuel P.; Nitschke, Jonathan R.; Journal of the American Chemical Society 137 (2015) 14502–14512; doi:10.1021/jacs.5b09920

data_4129725
_publ_section_title
;
 Stacking Interactions Drive Selective Self-Assembly and Self-Sorting of
 Pyrene-Based M(II)4L6 Architectures.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14502
_journal_page_last               14512
_journal_paper_doi               10.1021/jacs.5b09920
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'C240 H156 Fe4 N24, 8(C2 F6 N O4 S2), 3(C6 H6), C2 H3 N'
_chemical_formula_sum            'C276 H177 F48 Fe4 N33 O32 S16'
_chemical_formula_weight         6115.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.8510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7632(11)
_cell_length_b                   29.6794(14)
_cell_length_c                   45.408(2)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      94.819
_cell_measurement_theta_min      4.946
_cell_volume                     28981(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            77618
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        47.325
_diffrn_reflns_theta_max         47.325
_diffrn_reflns_theta_min         2.469
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.7493
_exptl_absorpt_correction_T_min  0.4548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             12448
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.574
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3278
_refine_ls_number_reflns         23817
_refine_ls_number_restraints     5939
_refine_ls_restrained_S_all      1.581
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.1398
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3816
_refine_ls_wR_factor_ref         0.4010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16065
_reflns_number_total             23817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09920_si_004.cif
_cod_data_source_block           jn1424_sq_d
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129725
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.813
_shelxl_version_number           2013-2
_shelx_res_checksum              16983
_shelx_hkl_checksum              86307