Control of Complex Formation through Peripheral Substituents in Click-Tripodal Ligands: Structural Diversity in Homo- and Heterodinuclear Cobalt-Azido Complexes.
Sommer, Michael G.; Marx, Raphael; Schweinfurth, David; Rechkemmer, Yvonne; Neugebauer, Petr; van der Meer, Margarethe; Hohloch, Stephan; Demeshko, Serhiy; Meyer, Franc; van Slageren, Joris; Sarkar, Biprajit; Inorganic chemistry 56 (2017) 402–413; doi:10.1021/acs.inorgchem.6b02330

data_4344968
_publ_section_title
;
 Control of Complex Formation through Peripheral Substituents in
 Click-Tripodal Ligands: Structural Diversity in Homo- and Heterodinuclear
 Cobalt-Azido Complexes.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              402
_journal_page_last               413
_journal_paper_doi               10.1021/acs.inorgchem.6b02330
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C60 H60 N23 Co2, 3(Cl O4), C2 N'
_chemical_formula_sum            'C62 H60 Cl3 Co2 N24 O12'
_chemical_formula_weight         1557.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.022(3)
_cell_length_b                   15.856(3)
_cell_length_c                   27.632(6)
_cell_measurement_reflns_used    19562
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      4.5
_cell_volume                     7280(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.1091
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            56229
_diffrn_reflns_theta_full        29.38
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         4.57
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.9047
_exptl_absorpt_correction_T_min  0.6073
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         19562
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2081
_refine_ls_wR_factor_ref         0.2371
_reflns_number_gt                10884
_reflns_number_total             19562
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b02330_si_002.cif
_cod_data_source_block           sarh83
_cod_depositor_comments
'Adding full bibliography for 4344962--4344968.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4344968