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_4340694
_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         '3(C15 H27 Co1 N4 O3), K3, 2(C3 H7 N O)'
_chemical_formula_sum            'C51 H95 Co3 K3 N14 O11'
_chemical_formula_weight         1374.5
_chemical_name_common            jb157
_chemical_name_systematic
;
 jb157
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
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_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2011-04-28T16:20:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                101.679(6)
_cell_angle_beta                 90.391(5)
_cell_angle_gamma                102.034(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4438(9)
_cell_length_b                   18.0953(16)
_cell_length_c                   18.3368(13)
_cell_measurement_reflns_used    217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3314.7(5)
_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 0.989
_diffrn_measured_fraction_theta_max 0.983
_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  0.2881
_diffrn_reflns_av_unetI/netI     0.2454
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            100643
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.9072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         12077
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.2159
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.134
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                5195
_reflns_number_total             12077
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5013389_si_001.cif
_cod_data_source_block           jb157
_cod_depositor_comments
'Adding full bibliography for 4340692--4340695.cif.'
_cod_database_code               4340694