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_4315866
_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            'C84 H79 Co3 N34 O5.5'
_chemical_formula_weight         1829.60
_chemical_name_systematic
; 
 ? 
;
_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                73.1710(10)
_cell_angle_beta                 74.4400(10)
_cell_angle_gamma                76.392(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1985(9)
_cell_length_b                   15.9576(15)
_cell_length_c                   16.0966(16)
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.426
_cell_measurement_theta_min      2.333
_cell_volume                     2146.6(4)
_computing_cell_refinement       'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_data_collection       'SMART Bruker AXS Inc., 1998.'
_computing_data_reduction        'SAINT+ Ver. 6.22, Bruker AXS Inc., 2001.'
_computing_molecular_graphics    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL Ver. 6.12, (Sheldrick, 2000)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex CCd'
_diffrn_measurement_method       'phi and omega 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11030
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.8447
_exptl_absorpt_correction_T_min  0.8197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1011P)^2^+1.0931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1925
_reflns_number_gt                4577
_reflns_number_total             7515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902548f_si_001_2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C84 H79 Co3 N34 O5.50'
_cod_database_code               4315866