DMF/H2O Volume Ratio Controls the Syntheses and Transformations of a Series of Cobalt Complexes Constructed Using a Rigid Angular Multitopic Ligand
Ai-Yun Fu; Yu-Lin Jiang; Yao-Yu Wang; Xiao-Nan Gao; Guo-Ping Yang; Lei Hou; Qi-Zhen Shi; Inorganic Chemistry 49 (2010) 5495–5502; doi:10.1021/ic902548f

data_4315865
_publ_contact_author_email       wyaoyu@nwu.edu.cn
_publ_section_title
;
 DMF/H2O Volume Ratio Controls the Syntheses and Transformations of a
 Series of Cobalt Complexes Constructed Using a Rigid Angular Multitopic
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5495
_journal_page_last               5502
_journal_paper_doi               10.1021/ic902548f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C36 H27 Co N15 O'
_chemical_formula_weight         744.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.1600(10)
_cell_angle_beta                 94.879(2)
_cell_angle_gamma                90.2000(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7316(9)
_cell_length_b                   12.7514(11)
_cell_length_c                   13.1627(12)
_cell_measurement_reflns_used    3239
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.523
_cell_volume                     1660.9(3)
_computing_cell_refinement       'SAINT (Bruker,1997)'
_computing_data_collection       'SMART (Bruker,1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8551
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.9609
_exptl_absorpt_correction_T_min  0.7662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.9464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                4681
_reflns_number_total             5820
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic902548f_si_001_1.cif
_cod_data_source_block           compound_4
_cod_database_code               4315865