Structural variability of Co(ii) and Ni(ii) entangled metal‒organic frameworks: effect of N-donor ligands and metal ions
Liu, Jian-Qiang; Wang, Yao-Yu; Huang, Yun-Sheng; CrystEngComm 13 (2011) 3733–; doi:10.1039/c0ce00871k

data_7205838
_publ_section_title
;
 Structural variability of Co(ii) and Ni(ii) entangled metal--organic
 frameworks: effect of N-donor ligands and metal ions
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3733
_journal_paper_doi               10.1039/c0ce00871k
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C84 H64 Co3 N6 O20'
_chemical_formula_sum            'C84 H64 Co3 N6 O20'
_chemical_formula_weight         1654.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 105.280(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.713(3)
_cell_length_b                   21.571(3)
_cell_length_c                   26.609(4)
_cell_measurement_reflns_used    8305
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.46
_cell_volume                     9254(3)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8305
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.46
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_correction_T_min  0.9373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Some residual electron density were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement.

There are two cavities cavities of 1275 \%A^3^ per unitl cell. PLATON
estimated that each cavity contains 37.5 electrons which may roughly
correspond to a mixture of solvent molecule of acetonitrile and water
molecule as suggested by chemical analyses.

;
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+0.0800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                4614
_reflns_number_total             8305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00871k.txt
_cod_data_source_block           aa
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7205838