Bifunctional pyrazolate‒carboxylate ligands for isoreticular cobalt and zinc MOF-5 analogs with magnetic analysis of the {Co4(μ4-O)} node
Heering, Christian; Boldog, Ishtvan; Vasylyeva, Vera; Sanchiz, Joaquín; Janiak, Christoph; CrystEngComm 15 (2013) 9757–; doi:10.1039/c3ce41426d

data_7238857
_publ_section_title
;
 Bifunctional pyrazolate--carboxylate ligands for isoreticular cobalt and
 zinc MOF-5 analogs with magnetic analysis of the {Co4(\m4-O)} node
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9757
_journal_paper_doi               10.1039/c3ce41426d
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H20 Co4 N6 O7'
_chemical_formula_sum            'C36 H20 Co4 N6 O7'
_chemical_formula_weight         884.30
_chemical_name_common            HHU-3
_space_group_IT_number           16
_space_group_name_Hall           'P 2 2'
_space_group_name_H-M_alt        'P 2 2 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2'
_symmetry_space_group_name_H-M   'P 2 2 2'
_atom_sites_solution_hydrogens   none
_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            1
_cell_length_a                   14.242(3)
_cell_length_b                   14.278(3)
_cell_length_c                   14.332(4)
_cell_measurement_reflns_used    1779
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      40.08
_cell_measurement_theta_min      3.09
_cell_volume                     2914.4(12)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6548
_diffrn_reflns_theta_full        40.08
_diffrn_reflns_theta_max         40.08
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    4.529
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains solvent molecules which have been treated as
a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.459(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                984
_reflns_number_total             1690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41426d.txt
_cod_data_source_block           p222p
_cod_original_cell_volume        2914.5(12)
_cod_original_sg_symbol_Hall     P22
_cod_original_sg_symbol_H-M      P222
_cod_database_code               7238857