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_4340693
_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         'C54 H60 Co N7 O3, C8 H20 N'
_chemical_formula_sum            'C62 H80 Co N8 O3'
_chemical_formula_weight         1044.27
_chemical_name_common            jb3_15
_chemical_name_systematic
;
 jb3_15
;
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_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_atom_sites_solution_secondary   difmap
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.269(3)
_cell_angle_gamma                90
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_cell_length_a                   18.9214(11)
_cell_length_b                   14.7819(10)
_cell_length_c                   20.8249(12)
_cell_measurement_reflns_used    715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5591.4(6)
_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 0.997
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            206671
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.36
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_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+3.3346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                11043
_reflns_number_total             13938
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5013389_si_001.cif
_cod_data_source_block           jb3_15
_cod_depositor_comments
'Adding full bibliography for 4340692--4340695.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4340693