Synthesis and reactivity of tripodal complexes containing pendant bases.
Blacquiere, Johanna M.; Pegis, Michael L.; Raugei, Simone; Kaminsky, Werner; Forget, Amélie; Cook, Sarah A.; Taguchi, Taketo; Mayer, James M.; Inorganic chemistry 53 (2014) 9242–9253; doi:10.1021/ic5013389

data_4340695
_publ_section_title
;
 Synthesis and reactivity of tripodal complexes containing pendant bases.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9242
_journal_page_last               9253
_journal_paper_doi               10.1021/ic5013389
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C27 H51 Co K N4 O9'
_chemical_formula_sum            'C27 H51 Co K N4 O9'
_chemical_formula_weight         673.75
_chemical_name_common            jb3_4
_chemical_name_systematic
;
 jb3_4
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-12-02T15:19:44-00:00
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9332(5)
_cell_length_b                   21.4229(12)
_cell_length_c                   16.8751(9)
_cell_measurement_reflns_used    345
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3229.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            110450
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.9516
_exptl_absorpt_correction_T_min  0.7391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.6
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+2.3773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.071
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                3469
_reflns_number_total             4266
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5013389_si_001.cif
_cod_data_source_block           jb3_4
_cod_depositor_comments
'Adding full bibliography for 4340692--4340695.cif.'
_cod_database_code               4340695