Coordination-Driven Self-Assembly of 2D-Metallamacrocycles Using a New Carbazole-Based Dipyridyl Donor: Synthesis, Characterization, and C60 Binding Study
Sankarasekaran Shanmugaraju; Vaishali Vajpayee; Sunmi Lee; Ki-Whan Chi; Peter J. Stang; Partha Sarathi Mukherjee; Inorganic Chemistry 51 (2012) 4817–4823; doi:10.1021/ic300199j

data_4328982
_publ_section_title
;
 Coordination-Driven Self-Assembly of 2D-Metallamacrocycles Using a New
 Carbazole-Based Dipyridyl Donor: Synthesis, Characterization, and C60
 Binding Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4817
_journal_page_last               4823
_journal_paper_doi               10.1021/ic300199j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C120 H86 Fe2 N6 P4 Pd2, C4 H10 O, 2(C F3 O3 S), C H3 N O2'
_chemical_formula_sum            'C127 H99 F6 Fe2 N7 O9 P4 Pd2 S2'
_chemical_formula_weight         2493.66
_chemical_name_systematic
; 
 ? 
;
_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                86.38(3)
_cell_angle_beta                 85.86(3)
_cell_angle_gamma                68.50(3)
_cell_formula_units_Z            2
_cell_length_a                   16.949(3)
_cell_length_b                   17.562(4)
_cell_length_c                   24.895(5)
_cell_measurement_reflns_used    22274
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      1.58
_cell_volume                     6871(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       'ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  'Diamond 3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.638
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'bending magnet 6B MX beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90000
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22274
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.8954
_exptl_absorpt_correction_T_min  0.7280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       blockshape
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1422
_refine_ls_number_reflns         11828
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1901P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2297
_refine_ls_wR_factor_ref         0.2431
_reflns_number_gt                8691
_reflns_number_total             11828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300199j_si_002_2.cif
_cod_data_source_block           Complex2a_m
_cod_original_cell_volume        6871(2)
_cod_database_code               4328982