Tris(2-pyridylborate) (Tpyb) Metal Complexes: Synthesis, Characterization, and Formation of Extrinsically Porous Materials with Large Cylindrical Channels
Chengzhong Cui; Patrick R. Shipman; Roger A. Lalancette; Frieder Jäkle; Inorganic Chemistry 52 (2013) 9440–9448; doi:10.1021/ic4010664

data_4335745
_publ_section_title
;
 Tris(2-pyridylborate) (Tpyb) Metal Complexes: Synthesis,
 Characterization, and Formation of Extrinsically Porous Materials with
 Large Cylindrical Channels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9440
_journal_page_last               9448
_journal_paper_doi               10.1021/ic4010664
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C50 H50 B2 Fe N6'
_chemical_formula_sum            'C50 H50 B2 Fe N6'
_chemical_formula_weight         812.43
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   35.4667(12)
_cell_length_b                   35.4667(12)
_cell_length_c                   9.8384(5)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.26
_cell_measurement_theta_min      2.49
_cell_volume                     10717.6(7)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.069
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18211
_diffrn_reflns_theta_full        64.11
_diffrn_reflns_theta_max         64.11
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             3852
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Total (Positive) Electron Count in Voids/Cell  =  111
Disordered solvent (cyclohexane) molecules were not determined, but 
SQUEEZE found that there were approximately two such disordered solvent 
molecules per cell.
;
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.50
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.98
_refine_ls_R_factor_all          0.074
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                2644
_reflns_number_total             3865
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic4010664_si_005.cif
_cod_data_source_block           complex2-Fe_C6H12
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4335745