Liquid-assisted solid-state reaction: assembly of (6,3) and (10,3) hydrogen-bonded networks based on [M(Hbiim)3] by oxidation of [M(H2biim)3]2+ complexes in the presence of acetate anions
Tan, Yu-Hui; Yang, Li-Fei; Cao, Man-Li; Wu, Jin-Ji; Ye, Bao-Hui; CrystEngComm 13 (2011) 4512–; doi:10.1039/c1ce00009h

data_7206171
_publ_section_title
;
 Liquid-assisted solid-state reaction: assembly of (6,3) and (10,3)
 hydrogen-bonded networks based on [M(Hbiim)3] by oxidation of
 [M(H2biim)3]2+ complexes in the presence of acetate anions
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              4512
_journal_paper_doi               10.1039/c1ce00009h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         '2(C18 H15 Co N12), 0.5(C4), H O '
_chemical_formula_sum            'C38 H31 Co2 N24 O'
_chemical_formula_weight         957.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6250(12)
_cell_length_b                   20.431(2)
_cell_length_c                   33.166(3)
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      1.23
_cell_volume                     8554.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28726
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_correction_T_min  0.7749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7213
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0764P)^2^+2.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                4996
_reflns_number_total             7213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce00009h.txt
_cod_data_source_block           complex_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        8555.0(14)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7206171