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_4129724
_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
'C228 H132 Co4 N36 O24, C2 F6 N O4 S2, 7(F6 P), 4(C6 H6), 2(C2 H3 N)'
_chemical_formula_sum            'C258 H162 Co4 F48 N39 O28 P7 S2'
_chemical_formula_weight         5684.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 91.101(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.1632(17)
_cell_length_b                   44.317(3)
_cell_length_c                   29.6106(15)
_cell_measurement_reflns_used    9362
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      88.693
_cell_measurement_theta_min      4.883
_cell_volume                     35638(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0391
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            91610
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        44.490
_diffrn_reflns_theta_max         44.492
_diffrn_reflns_theta_min         2.229
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.527
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.5699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       prism
_exptl_crystal_F_000             11536
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.440(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4883
_refine_ls_number_reflns         49795
_refine_ls_number_restraints     11352
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1979P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2479
_refine_ls_wR_factor_ref         0.2714
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                34068
_reflns_number_total             49795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09920_si_003.cif
_cod_data_source_block           jn1413_sq_d
_cod_original_cell_volume        35639(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4129724
_shelx_estimated_absorpt_t_min   0.538
_shelx_estimated_absorpt_t_max   0.645
_shelxl_version_number           2014/6
_shelx_res_checksum              70966
_shelx_hkl_checksum              9930