Highly Tunable Heterometallic Frameworks Constructed from Paddle-Wheel Units and Metalloporphyrins
Barron, Paul M.; Son, Hyun-Tak; Hu, Chunhua; Choe, Wonyoung; Crystal Growth & Design 9 (2009) 1960–; doi:10.1021/cg801267m

data_4509346
_publ_section_title
;
 Highly Tunable Heterometallic Frameworks Constructed from Paddle-Wheel
 Units and Metalloporphyrins
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1960
_journal_paper_doi               10.1021/cg801267m
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C68 H40 Fe N8 O8 Co2, (N O3)'
_chemical_formula_sum            'C68 H40 Co2 Fe N9 O11'
_chemical_formula_weight         1332.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.6367(16)
_cell_length_b                   16.6367(16)
_cell_length_c                   24.779(3)
_cell_measurement_reflns_used    7365
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.39
_cell_volume                     6858.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37396
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.8775
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    0.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1358
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Disordered, independent solvent molecules were eliminated from the refinement 
using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13].

R factors before data are squeezed:
_refine_ls_R_factor_all           0.0948 
_refine_ls_R_factor_gt            0.0859 
_refine_ls_wR_factor_ref          0.3255 
_refine_ls_wR_factor_gt           0.2936 
;
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1950
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1520P)^2^+5.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2079
_reflns_number_gt                1725
_reflns_number_total             1950
_reflns_threshold_expression     >2/sI
_cod_data_source_file            cg801267msup1.cif
_cod_data_source_block           C7CH33sq
_cod_original_cell_volume        6858.2(13)
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               4509346